Wood Sci Technol (2010) 44:421–433

DOI 10.1007/s00226-010-0361-3

ORIGINAL

Evaluation of thermally modified beech and spruce

wood and their properties by FT-NIR spectroscopy

Helmut Bächle • Bernhard Zimmer •

Elisabeth Windeisen • Gerd Wegener

Received: 15 April 2010 / Published online: 10 July 2010

Ó Springer-Verlag 2010

Abstract Quality assessment of thermally modified spruce (Picea abies (L.)

Karst) and beech (Fagus sylvatica L.) wood and of the corresponding reference
samples was carried out by means of non-destructive FT-NIR spectroscopic mea-
surements and PLS regression. Oven-dry and basic density as well as MOE and
MOR determined by 3-point bending tests were evaluated. The focus was put on
specimens produced from material that had been thermally modified in an industrial
scale kiln. Modelling results range from poor to very good. The results of the spectra
taken from the spruce samples resulted in better prediction results than the spectra
of the beech samples. This could be due to different proveniences or variation in the
industrial modification process. The results indicate that FT-NIR surface measure-
ments of sound thermally modified wood samples could be applied to evaluate
several characteristics before and after the modification process. The method could
be used for screening during pre-sorting of thermally modified wood.

Introduction

Thermal treatment of wood as a modification method and the production of

thermally modified timber (TMT) have increased significantly during the last
decade (Hill 2006). Major applications of TMT are, for example, garden furniture
and deckings for terraces, spa areas or swimming pools and floorings. The effects of
temperature on wood properties have been studied since the beginning of the 20th

H. Bächle (&)
E. Windeisen
G. Wegener

Holzforschung München, Technische Universität München, Winzererstr. 45,
80797 Munich, Germany
e-mail: baechle@wzw.tum.de

B. Zimmer
Salzburg University of Applied Sciences, Markt 136a, 5431 Kuchl, Austria

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century. Many studies quantify the effect of thermal modification on the properties
of wood (Hill 2006, Esteves and Pereira 2009, and literature cited therein).
However, there are still several problems to be solved. Among them are varying
material properties due to a number of industrial thermal treatment processes.
Although first efforts for standardization have been made (CEN/TS 15679), there is
still a lack of fast and efficient quality control methods. Thus, major ambitions of
producers and customers have been the establishment of cost-effective quality
control and assurance methods (Scheiding 2008).
Since wood becomes darker with increasing treatment time and temperature,
colour measurement has been suggested for quality control of TMT. Studies on the
relationship between colour changes and wood properties, especially strength, are
contradictory. Bekhta and Niemz (2003) reported a strong relationship between
colour change and strength of thermally treated spruce samples. Gonzalez-Peña and
Hale (2009) successfully predicted the changes of several properties of beech,
Norway spruce and Scots pine specimens by means of different regression analyses
of colour changes, and Brischke et al. (2007) found a correlation between colour
measured on homogenized wood samples and mass loss. However, Johansson and
Moren (2006) reported that colour is not a suitable predictor of strength in thermally
modified birch wood. Schnabel et al. (2007) reported about an approach to classify
thermally treated hardwoods by determining the colour.
Within the last two decades, near-infrared spectroscopy (NIRS) has been
recognized as one of the most powerful non-destructive techniques for wood
analysis. Multivariate statistical methods such as principal component analysis
(PCA), principal component regression (PCR) and partial least-square regression
(PLSR) were developed as standard methods for the evaluation of NIR spectra. In
contrast to colour measurements, the characterization of mechanical properties of
wood by NIRS has been reported in numerous studies (So et al. 2004, Tsuchikawa
2007, and literature cited therein).
The application of NIRS on TMT for classification purposes was suggested by
Hinterstoisser et al. (2003). They analysed thermally treated Norway spruce samples
(Picea abies (L.) Karst.) by analysing wood meal taken from the sample surface.
The samples were treated for 0–48 h at a temperature of 167°C (440 K). Small
differences were observed for samples treated between 3 and 9 h. However, the
spectral differences between the 18 and 48 h treatments were obvious. Schwann-
inger et al. (2004) reported a close relationship between the chemical changes of
thermally modified Fagus sylvatica L. samples and the corresponding NIR spectra,
while Mitsui et al. (2008) observed thermally induced alterations of the phenolic
and cellulosic hydroxyl groups of Picea sitchensis. Esteves and Pereira (2008)
predicted the properties of pine (Pinus pinaster Labill.) and eucalypt (Eucalyptus
globulus Aiton) by analysing the radial surface of the samples using a NIR fibre
probe. The thermal treatment was conducted in a laboratory oven at 170–210°C for
2–24 h and in an autoclave at 190–210°C for 2–12 h. The calibration models are
reported to be good for cross-validation results, with coefficients of determination
ranging between 96 and 98% for mass loss, 78 and 95% for equilibrium moisture
content, 53 and 78% for dimensional stability, 47 and 89% for MOE, 75 and 77%
for bending strength.

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Thus, NIRS has the potential to be used in quality control of thermally modified
wood. It allows for evaluation of several wood properties by measuring one single
spectrum. In this study, NIRS and multivariate chemometric methods were used to
evaluate modulus of rupture (MOR), modulus of elasticity (MOE), density and
moisture content of beech (Fagus sylvatica L.) and Norway spruce (Picea abies (L.)
Karst) wood after thermal modification in an industrial scale kiln.

Materials and methods

Material

Beech (Fagus sylvatica L.) and Norway spruce (Picea abies (L.) Karst.) samples
were analysed. The beech samples consisted of two sets. One sample set was
modified and cut in 2003. The second sample set was thermally modified in 2007.
Matched samples were cut from two boards per stem containing the pith (Fig. 1).
One board was thermally modified, and the other board was used as untreated
reference material. The boards prepared in 2003 were cut from trees showing
between 81 and 160 growth rings. The boards from 2007 had about 85 growth rings.
Table 1 presents the number of trees used for each sample set and the treatment
intensity. For the preparation of the spruce samples, only one board per stem
containing the pith was used. The boards were longitudinally cut into four sections
prior to thermal treatment (Fig. 1).
Prio to the bending test, samples were cut, and the boards were divided into zones
on the cross-section, each 30 growth rings wide. Material within the first 30 growth
rings around the pith was not used for analyses due to the influence of juvenile wood
and the concentration of cracks after modification in this zone.
The bending test samples were cut from the middle of the growth ring zone to
provide comparable samples in the longitudinal direction. Specimens containing
knots or visible cracks were discarded.

Fig. 1 Schema of sample treatment of beech and spruce boards

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Table 1 Number of trees used

Beech Spruce
for sample preparation
Year 2003 2006 2007

Reference 23 6 17
180°C 7 2 17
200°C 9 2 17
220°C 7 2 17

Thermal treatment was conducted in an industrial scale kiln at 180, 200 and
220°C for 4 h under oxygen exclusion by the evolving wood gas.

Mechanical testing

Mechanical testing was conducted on a Zwick Roell Z250 universal testing

machine. MOE and MOR were determined by a three-point bending test with
specimens measuring 20 mm 9 20 mm 9 360 mm according to DIN 52186
(1978). MOE was calculated between 100 and 500 N, which was about 5–50% of
the maximum load depending on the species and the treatment intensity. Oven-dry
(o.d.) and basic density were determined gravimetrically according to DIN 52182
(1976) subsequent to the bending tests.

NIR spectroscopy

NIR diffuse-reflectance spectra were collected using a FT-NIR spectrophotometer

(Bruker MPA) and the Bruker software OPUS 5.5. The NIR spectra were acquired
by an integrating sphere scanning an area of about 1 cm in diameter. Thirty-two
scans were averaged per scan at a spectral resolution of 8 cm-1 between 10,000 and
4,000 cm-1. Seven spectra on the radial longitudinal face of bending test samples
were averaged to one average spectrum per face. The measurements were taken on a
planed surface under laboratory conditions.

Data processing

Unscrambler 9.6 (Camo) software was used for data pre-processing and for
computing of calibration and prediction models. First derivative was obtained by
using a 9-point filter and a second order polynomial as well as the Savitzky-Golay
algorithm (Savitzky and Golay 1964). For the 2nd derivative, a 15-point filter and a
second order polynomial were used. Furthermore, standard normal variate
transformation (SNV) was applied.
The samples were divided into two sets. About two-third of the specimens were
used for calculating the calibration models, while about one-third was used as a test
set for validation purposes. Furthermore, the samples were divided into a set
consisting of the reference samples and a set of TMT samples. A third set comprised
all reference and TMT samples (TMT/Reference) of a species. Calibrations were
developed using the partial least-squares regression (PLS regression) method

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provided by the Unscrambler 9.6 software package. A detailed description of PLS

regression is given by Esbensen (2002) and Kessler (2007). The calibration models
were developed in cross-validation mode with a maximum of ten latent variables
(LV). The final number of LVs adopted for the models corresponded to the first
minimal residual variance. The calibration models were validated by an independent
test set. Outlier samples were identified by Student residuals and leverage value plot
analyses. Standard error of calibration (SEC) and R2cal was used to assess calibration
performance. The standard error of prediction (SEP) shows how well the calibration
model predicts the parameter investigated for an unknown sample set. The ratio of
performance to deviation (RPD) was calculated as suggested by Williams and
Norris (2001). It is calculated as the ratio of the standard deviation of the reference
data to SEP. The RPD value is a basis for standardizing the SEP and comparing the
performance of different models. For screening purposes, a RPD of at least 2.5 is
suggested to be satisfactory. Dependent on the application, a RPD of more than 1.5
can be satisfactory for initial screening (Williams and Norris 2001).

Results and discussion

NIR spectra

Averaged and normalized NIR spectra of spruce samples before and after thermal
treatment are presented in Fig. 2. The overlapping absorption bands were resolved
by calculating the 2nd derivatives (Figs. 3 and 4). The baseline shift of the raw
spectra towards higher wave numbers is due to the darker colour of the treated
samples. Below 7,100 cm-1, the baseline shift is induced by the density change
caused by the mass loss due to the degradation of the cell wall polymers. The
decrease in absorption at the water OH band at 5,150 cm-1 with treatment intensity

0.7

0.6

5150
0.5
Absorption

0.4

0.3
8300
0.2

0.1

0
9000 8000 7000 6000 5000 4000
Wavenumber [1/cm]
Spruce reference Spruce 180°C Spruce 200°C Spruce 220°C

Fig. 2 Normalized NIR spectra of spruce samples before and after thermal treatment

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1.00E-004

log (1/R) - 2nd derivative

5.00E-005

5865
0.00E+000 5800
5981

-5.00E-005

-1.00E-004

-1.50E-004
6000 5950 5900 5850 5800 5750 5700
Wavenumber [1/cm]
Spruce reference Spruce 180°C Spruce 200°C Spruce 220°C

Fig. 3 Second derivative of NIR spectra of spruce samples before and after thermal treatment between
5,700 and 6,000 cm-1

8.00E-005

6.00E-005
log (1/R) 2nd derivative

4.00E-005
6460
2.00E-005 6900 6722

0.00E+000
7000
-2.00E-005

-4.00E-005

-6.00E-005

-8.00E-005

-1.00E-004
7150 7050 6950 6850 6750 6650 6550 6450
Wavenumber [1/cm]
Spruce reference Spruce 180°C Spruce 200°C Spruce 220°C

Fig. 4 Second derivative of NIR spectra of spruce samples before and after thermal treatment between
6,450 and 7,200 cm-1

is related to the lower moisture content of the samples after thermal treatment. At
around 8,300 cm-1, the absorption of the second overtone of CH stretching
vibrations decreases. This is caused by the degradation of carbohydrates and
deacetylation reactions of the polyoses and can also be seen by the alterations of
absorption at the CH stretching vibration first overtone band at 5,800 and
5,865 cm-1 (Fig. 3). At the OH stretching vibration absorption bands of the
amorphous (7,000 cm-1), semi-crystalline (6,722 cm-1) and crystalline
(6,460 cm-1) regions of cellulose (Tsuchikawa and Siesler 2003), differences
before and after thermal treatment can be observed (Fig. 4) that might be attributed
to the cleavage of OH groups during thermal treatment (Mitsui et al. 2008).
Although lignin is supposed to be comparatively stable at higher temperature, the

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skeletal CH absorption band at 5,981 cm-1 (Mitsui et al. 2008) features differences,
which indicate modifications in lignin after thermal treatment. At 6,900 cm-1, the
cleavage of aromatic OH groups originating from lignin causes spectral differences
in the second derivative (Fig. 4). The NIR spectra of the beech samples (Windeisen
et al. 2009) show features similar to the spectra of the spruce specimens. However,
the differences of the beech spectra before and after thermal treatment seem to be
more obvious at the corresponding treatment intensity (e.g., in the region of CH first
overtone vibration between 5,500 and 6,000 cm-1). This might be attributed to the
differences of the chemical composition of softwood and hardwood. Due to
the lower content of acetyl groups in softwoods, less acetic acid, that catalyses the
degradation of carbohydrates during the thermal modification, is released resulting
in a lower mass loss of the spruce samples. Furthermore, softwood contains less
easily degradable polyoses.

PLS regression

Density

The calibrations developed for basic and oven-dry density, and the results when the
calibrations were applied to predict the density of the test set samples are shown in
Table 2. Figures 5 and 6 present the measured vs. predicted oven-dry density of
Norway spruce and beech TMT/Reference datasets. Best calibration results were
achieved for spruce reference samples. R2cal was 0.95 (basic density) and 0.91 (oven-
dry density), the corresponding SEC was 0.01 g/cm3. R2TS of the prediction results
was 0.79 and 0.70, and the SEP was 0.02 g/cm3. The statistics for the beech
references was lower except for the prediction of oven-dry density (R2TS = 0.71).
However, RPD of the spruce references is slightly lower than the one of the beech
references. It ranges from 1.67 to 2.04.
The statistics of the TMT spruce models show lower R2 and higher standard
errors. The beech TMT samples calibration models performed slightly better than
the reference sample sets. However, the corresponding prediction results of the
TMT specimens are poorer than those of the reference sets. The number of LVs was
6–10 except for the beech references where 3 (basic density) LVs were used.
The combined sample sets (TMT/Reference) of spruce showed R2 values greater
than the corresponding TMT models and lower than the reference models. The
beech calibration sample sets showed a different tendency since the results of
reference calibration performed lower R2cal than the TMT calibrations. The
prediction models of beech, however, correspond to the behaviour of the spruce
samples.
RPD was between 1.5 and 2.0 for all data sets except for basic density of the
spruce TMT samples (1.4).

Mechanical properties

The evaluation of mechanical properties of wood is of crucial importance since

experimental destructive testing requires time-consuming and expensive methods.

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Table 2 Summary statistics of the calibration and validation models for MOE, MOR, basic and oven-dry
density for thermally modified beech and spruce samples, the corresponding reference samples and the
combined sample sets based on NIR spectral measurements
Pre-treatm.* LV’s No. of R2cal SEC No. of R2TS SEP RPD
samples samples

MOE
Spruce
TMT/reference 2ndDer 7 183 0.84 833.63 88 0.66 1,077.10 1.73
Reference 2ndDer 7 56 0.98 390.63 25 0.68 938.07 1.67
TMT raw 10 128 0.75 912.26 62 0.75 989.74 1.99
Beech
TMT/reference 1stDer 7 216 0.50 1,025.40 106 0.47 978.77 1.39
Reference 2ndDer 6 78 0.72 592.35 34 0.36 863.87 1.32
TMT 1stDer 8 134 0.59 958.81 66 0.38 1,061.88 1.27
MOR
Spruce
TMT/reference 2ndDer 6 183 0.56 13.01 86 0.43 14.07 1.33
Reference 2ndDer 8 55 0.99 1.76 24 0.59 6.20 1.52
TMT 2ndDer 5 128 0.52 14.38 62 0.46 15.56 1.36
Beech
TMT/reference 2ndDer 6 217 0.62 15.50 106 0.55 16.82 1.50
Reference raw 9 76 0.38 8.86 34 0.16 9.56 1.10
TMT norm. 6 135 0.66 19.20 71 0.57 18.82 1.52
Basic density
Spruce
TMT/reference 1stDer 9 186 0.75 0.02 88 0.63 0.02 1.64
Reference 1stDer 10 56 0.95 0.01 24 0.79 0.02 1.97
TMT 1stDer 8 129 0.69 0.02 62 0.58 0.03 1.52
Beech
TMT/reference 1stDer 10 218 0.70 0.03 106 0.57 0.03 1.57
Reference 1stDer 6 78 0.67 0.03 34 0.72 0.03 2.04
TMT 2ndDer 8 138 0.73 0.03 72 0.54 0.04 1.35
Oven-dry density
Spruce
TMT/reference 1stDer 9 187 0.73 0.02 86 0.62 0.02 1.62
Reference norm. 10 56 0.91 0.01 24 0.70 0.02 1.69
TMT 1stDer 8 129 0.68 0.02 62 0.57 0.02 1.52
Beech
TMT/reference raw 8 189 0.68 0.03 90 0.69 0.03 1.81
Reference 2ndDer 3 68 0.67 0.03 29 0.71 0.03 1.88
TMT 1stDer 8 122 0.77 0.03 65 0.65 0.03 1.74

* Pre-treatment
raw no spectral treatment, norm. normalization, 1stDer 1st derivative, 2ndDer 2nd derivative

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Fig. 5 Measured vs. predicted values of oven-dry (o.d.) density, MOE and MOR of calibration and
validation from TMT/reference samples of Norway spruce

Several models for the prediction of mechanical properties by NIR spectra were
developed for thermally treated wood and its references. Table 2 presents the results
of the best models for MOE and MOR of thermally treated beech and spruce
specimens and their corresponding references.
The calibration and validation statistics of MOE of the spruce sample sets are
moderate to very good, achieving R2cal values between 0.75 (TMT) and 0.98

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Fig. 6 Measured vs. predicted values of oven-dry (o.d.) density, MOE and MOR of calibration and
validation from TMT/reference samples of beech

(reference), R2TS between 0.66 and 0.75, SEC between 391 N/mm2 (reference) and
912 N/mm2 (TMT) and SEP between 938 N/mm2 (reference) and 1,077 N/mm2
(TMT/Reference). The number of latent variables was 7 for the reference and TMT/
Reference set and 10 for the TMT specimens. R2cal was good to very good (0.75–
0.98) while the test set validation achieved moderate to good R2TS (0.66–0.75). RPD
ranged from 1.67 (reference) to 1.99 (TMT).

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The beech sample models performed worse than the spruce sample models. R2cal
was between 0.50 (TMT/Reference) and 0.72 (reference), while R2TS of the
validation ranged from 0.36 (reference) to 0.47 (TMT/Reference). SEC and SEP
were between 592 N/mm2 and 1,025 N/mm2 and between 864 N/mm2 and 1,062 N/
mm2. Due to a lower range of MOE for the beech samples a lower SEC and SEP
compared to the spruce samples could be expected. However, this was not the case.
Considering the greater standard deviation of MOE for the spruce samples, the
resulting RPD for the beech (1.27–1.39) samples is lower than those of the spruce
samples and \1.5 for all beech models.
Predicted vs. measured values of MOE and MOR of TMT/Reference data sets are
plotted in Figs. 5 and 6. Some samples (especially beech) show a considerable
distance from the regression line and, thus, had a higher contribution to SEC/P.
Considering MOR, the spruce specimens achieved moderate to very good
calibration results with R2cal of 0.52 and 0.56 for TMT and TMT/Reference samples
and 0.99 for the reference data. LVs for TMT sample sets were lower than those of
MOE. For the reference samples, one more LV (8) was used. SEC ranged from 2 N/
mm2 (reference) to 14 N/mm2 (TMT). R2TS values of the MOR were moderate and
ranged from 0.43 (TMT/Reference) to 0.59 (TMT). RPD was generally poor
ranging between 1.33 and 1.52. The beech reference samples achieved very poor
results. R2 of calibration was 0.32 and of validation 0.16. The corresponding RDP is
1.1. This is surprising, since the models of the reference samples of spruce and ash
(Bächle et al. 2009) perform best. One reason might be the composition of the data
set of the beech samples. The samples consisted of two batches assumingly from
different proveniences. There were visible differences in structure on the radial and
tangential face (e.g., height of rays). Besides, density and standard deviation were
different.
Generally, a great variation of the measured parameters could be observed
resulting in high coefficients of variation for the calibration and the validation data
sets. The standard deviations of MOE and MOR of the TMT samples are in line
with the results of Esteves and Pereira (2008) for pine (Pinus pinaster) and eucalypt
wood (Eucalyptus globulus). The variation of calibration and validation sets within
the TMT data was higher than the ones of the reference data. This could be observed
by higher coefficients of variation for the TMT data. By combining the reference
and the TMT samples, the variation was lower compared to the TMT data and
higher compared to the reference data. Thus, the models of the combined data sets
performed in general better than the TMT sets but poorer than the reference sets.
The TMT specimens were produced under industrial conditions in an industrial
scale kiln. Experiments have shown that treatment conditions in the laboratory are
more stable than in industry. This might lead to higher variation of the sample
material and might be co-responsible for the lower performance of the TMT models,
especially those of beech.
Various parameters might influence the measurements. NIR spectra are very
sensitive to moisture over the whole spectral range and colour at higher
wavenumbers. For the acquisition of the NIR spectra, 32 scans per spectrum were
taken. Esteves and Pereira (2008) measured 50 scans and Gindl et al. (2001) 100
scans. Better statistics might be achieved if more scans per spectrum were taken.

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However, this means a more time-consuming acquisition, which was the reason in
this study for acquiring 32 scans and averaging seven spectra per face and sample. A
further inquiry of the relation between the number of scans, resolution and the
number of spectra averaged per sample might offer more information about the
spectra acquisition optimum for solid wood samples.
The distribution of the measured values for each parameter was not ideally
equally distributed. The effect can be observed in Figs 5 and 6. The results of
prediction at high values tend to appear lower, while those at the lower end tend to
appear higher than the actual measured values.

Mathematical treatments

First and 2nd derivatives of the NIR spectra provided the best modelling results in
most cases when applied to the spectra measured on the radial longitudinal face.
SNV and normalization proved to be best in individual cases. However, the results
were only slightly better than those of the 1st or 2nd deviation.

Conclusion

The results presented in this study demonstrate that it is possible to develop general
calibrations for small sound TMT specimens produced in an industrial kiln. The low
performance of NIR spectra of beech samples might at least partly be related to
different proveniences and/or the industrial processing environment. Thus, the
variations induced by different geographical origins and industrial processes need to
be considered during calibration phase. RPD values of TMT sample containing data
sets indicate that the models could be at least used for rough screening. Considering
the variability of wood and the statistics of traditional sorting methods, the results
indicate that NIRS in combination with PLS regression is suitable for estimating
density, MOE and MOR of industrially produced TMT samples especially when
mixed TMT/reference calibration models are used. Thus, NIRS measurements of
the wood solid surface might be applied to estimate several characteristics that can
be related to the properties before and after thermal treatment. An application
focussed pre-sorting system for TMT samples might be based on NIR spectroscopy.
However, further investigations based on large scale samples are necessary.

Acknowledgments The investigations were funded by the Austrian Research Promotion Agency (FFG)
in the program line ‘‘FHplus’’ (No. 811968).

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