Fuel 90 (2011) 2321–2325

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Fuel
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Visible and NIR Spectroscopy to assess biodiesel quality: Determination

of alcohol and glycerol traces
M. Pilar Dorado a,⇑, Sara Pinzi a, Antonio de Haro b, Rafael Font b, Juan Garcia-Olmo c
a
Department of Physical Chemistry and Applied Thermodinamics, Ed Leonardo da Vinci, Campus de Rabanales, 14071 Cordoba, Spain
b
Department of Agronomy and Plant Breeding, IAS-CSIC, Alameda del Obispo s/n, 14080 Cordoba, Spain
c
NIR/MIR Spectroscopy Unit, Central Service for Research Support (SCAI), University of Cordoba, Campus de Rabanales, 14071 Cordoba, Spain

a r t i c l e i n f o a b s t r a c t

Article history: Biodiesel quality control is of relevant importance as biodiesel properties influence diesel engine perfor-
Received 11 December 2010 mance. In the present work, the benefits of the use of visible and near-infrared Spectroscopy (NIRS) as a
Received in revised form 8 February 2011 technique for screening undesirable contaminants, i.e. methanol and glycerol content in biodiesel are
Accepted 15 February 2011
presented. Excess of methanol decreases heating value and flash point and increases carbon deposits,
Available online 22 March 2011
while the presence of glycerol may cause injector tip coking and deposits in the combustion chamber.
Biodiesel samples contaminated with different amounts of methanol and glycerol were scanned by NIRS.
Keywords:
Their NIR spectra were acquired at 2-nm intervals over a wavelength range from 400 to 2500 nm (visible
NIRS
Visible region
plus near-infrared regions). First derivative of the spectra were calculated and correlated to the raw opti-
Glycerol detection cal data by means of modified partial least-squares (MPLS) regression. First derivative equation of the
Methanol detection optical data, pretreated by standard normal variate (SNV) and De-trending (DT) transformations, showed
Biodiesel standard a coefficient of determination r2 in the cross-validation step of 0.99 and 0.81, for the samples contami-
nated with methanol and glycerol, respectively. Also, the standard deviation to standard error of cross-
validation ratio (RPD) was 10.0 and 2.5, respectively. These statistics are indicative of the high capacity
of prediction of the equations for methanol content and acceptable for glycerol content. Visible spectra
also showed differences related to the samples, thus indicating it could serve to determine the presence
of these contaminants. The use of NIRS technology provides a trustworthy and low-cost method to deter-
mine the presence of undesirable amounts of methanol and glycerol. It also offers an important saving of
time (each analysis requires less than two minutes).
Ó 2011 Elsevier Ltd. All rights reserved.

1. Introduction
Increasing environmental concerns are leading energy policies
to promote research in the field of new alternative fuels, among
them is biodiesel. Biodiesel is a fuel produced via transesterifica-
tion of fatty acids from vegetable oils or animal fats, moreover con-
sidered renewable energetic sources [1]. Thus, the use of biodiesel
in diesel engines reduces exhaust emissions, while engine perfor-
mance remains constant or slightly decreases compared to the
use of diesel fuel [2,3]. The most popular raw materials used to
produce biodiesel are rapeseed oil (center of Europe), sunflower
oil (south of Europe), soybean oil (US) and used frying oils from dif-
ferent origins [4].
Presence of pollutants in biodiesel (residual alcohol, unreacted
glycerides, free fatty acids, glycerol, moisture) can produce severe
engine problems. In fact, excess of alcohol facilitates the formation
of large carbon deposits in the engine, as well as lacquer deposits
⇑ Corresponding author. Tel.: +34 957 218332; fax: +34 957 218417.
E-mail address: qf1dopem@uco.es (M. Pilar Dorado).
on the injector tips [5]. Moreover, increasing the presence of alco-
hol decreases biodiesel heating value, while increases fuel con-
sumption, pressure and delays ignition, thus decreasing engine
power and energetic content [6]. Furthermore, residual alcohols
in biodiesel decrease initial temperature of the distillation curve
as well as flash point, due to its volatility, causing problems during
start-up in cold weather [7]. On the other hand, excess of alcohol in
the presence of excess of catalyst inhibits complete separation of
glycerol from biodiesel [1]. Furthermore, excess of alcohol in-
creases biodiesel production cost, thus the use of the exact amount
of alcohol to reach the maximum ester yields is recommended.
Glycerol residues must also to be taken into consideration. Excess
of glycerol can cause problems during storage and inside engine
fueling system. Deposits caused by contamination by glycerine will
cause injector tip coking and deposits in the combustion chamber.
This can increase aldehydes emissions and produce injection sys-
tem corrosion [8]. For these reasons, quality control tests are
needed. In fact, biodiesel European standard EN 14214 limits the
presence of some pollutants, among them are alcohol and free
glycerol.

0016-2361/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.fuel.2011.02.015
2322 M. Pilar Dorado et al. / Fuel 90 (2011) 2321–2325

Heretofore, the assessment of biodiesel quality has been con-
ducted by gas chromatography (GC) and high-performance liquid
chromatography (HPLC) [9,10]. A method via GC for analyzing
mono-, di-, triacylglycerides, methyl esters and glycerol in one
run was developed [11]. Darnoko et al. [12] and Arzamendi et al.
[13] developed size exclusion chromatography (SEC) methods in
order to monitor glyceride contents and FAME yield during biodie-
sel production. Pinzi et al. [14] developed an ultrasound assisted
automatic on-line method for the determination of bounded and
free glycerol in biodiesel.
On the other hand, near infrared spectroscopic (NIRS) methods
for quality control have been reported. NIRS is a technique that uses
the radiation absorbed by a set of samples in a region from 700 to
2500 nm to develop calibration curves related to sample properties.
After calibration, the regression equation permits fast analysis of
many other samples by prediction of data on the basis of the spec-
tra. The most attractive features of NIRS analysis are measurement
speed, minimal sample preparation and non-destructiveness, mak-
ing it possible to conduct large numbers of analyses in a short time.
NIRS has been widely used for the last decades as fast and accurate
method for qualitative and quantitative analysis of biological and
non-biological materials in different fields. Petrochemical industry
has used NIRS to analyze petroleum derivatives and properties,
quality of lubricants and other by-products, to predict physical
properties of mixtures of hydrocarbons, etc. [15–17]. This method-
ology could help to improve the quality control process related to
both biodiesel production and testing. In fact, Knothe successfully
monitorized for completion the transesterification reaction, as-
sessed biodiesel quality through the NIR method and determined
the blend level of biodiesel in conventional diesel fuel [18,19]. Fur-
thermore, Felizardo et al. [20] reported the development of calibra-
tion models for water and methanol in biodiesel, whereas Baptista
et al. developed calibration models to predict total methyl ester and
principal fatty acid contents in biodiesel [21] and other biodiesel
quality parameters such as iodine value, CFPP, kinematic viscosity
and density [22]. However, compared to other techniques, NIRS is
a relative methodology, so calibration samples must be previously
analyzed using a reference method. It is not selective, so multivar-
iate analysis has to be used to extract relevant information and it is
necessary to obtain a large number of samples to develop robust
calibration equations.
The target of this work was to assess the suitability of NIRS and
visible spectra to determine methanol and glycerol traces in bio-
diesel. As far as we know, only NIR wavelength range has been
used to determine biodiesel quality. However, visible region could
provide valuable information about the same topic, thus decreas-
ing costs.
2. Materials and methods
2.1. Raw materials
Biodiesel from used oil, complying with biodiesel fuel specifica-
tions according to European standard EN 14214, was supplied by
Stocks del Vallès, S.A. (Llerona, Spain). Some biodiesel properties
are given in Table 1. Methanol for analysis, ACS-ISO and glycerol
PA-ACS-ISO were acquired from PANREAC QUÍMICA SA (Barcelona,
Spain).
2.2. NIRS analysis
A set of 50 biodiesel samples was contaminated with methanol
(subset 1) in a range from 0.003% to 0.433% m/m. A set of 25 bio-
diesel samples was contaminated with glycerol (subset 2) in a
range from 0.005% to 0.050% m/m. Both ranges were chosen in or-
der to include the maximum authorized value for methanol and
glycerol residues, respectively, according to the European biodiesel
standard EN 14214. Each sample (10 ll volume) was placed in the
NIRS gold sample holder (3 cm diameter). The lens holder has an
anodized aluminum base made of crystal quartz. Samples were
scanned in a NIR spectrometer (NIRSystems model 6500,
Foss-NIRSystems, Inc., Silver Spring, MD, USA) in double transmit-
tance mode, equipped with a transport module, acquiring their NIR
spectra at 2 nm intervals over a wavelength range from 400 to
2500 nm (visible together with NIR regions).
Using the WinISI II v. 1.50 program (Infrasoft International, LLC,
Port Matilda, PA, USA), different calibration equations for the
methanol and glycerol content were developed on both calibration
sets. Each NIR spectrum was correlated to the each sample with
different content of methanol or glycerol, so two matrices contain-
ing the spectral values as the independent variable, and the values
of methanol or glycerol as the dependent variable, were generated.
Calibration equations were computed using first derivative of the
optical data (log(1/R), where R is reflectance), with a standard nor-
mal variate (SNV) and De-trending (DT) mathematical pretreat-

Table 1
Biodiesel properties.

Parameter Method Unit Result Biodiesel European standard EN 14214:2008

3
Density at 15 °C ISO 3675 kg/m 883.9 860–900
Viscosity at 40 °C EN ISO 3104 mm2/s 4.64 3.5–5.0
Flash point EN ISO 22719 °C 176 >101
CFPP EN 116 °C 2 <0 (it depends on the climate)
Sulfur content EN ISO 20846 % m/m 0.0015 <0.01 (10 mg/kg)
Carbon residue (original) EN ISO 10370 % m/m 0.02 <0.3
Cetane number FIA 100 – 67 >51.0
Sulfated ash ISO 3987 % m/m <0.01 <0.02
Water content EN ISO 12937 mg/kg 7 <500
Total contamination EN 12662 mg/kg 1 <24
Corrosivity to copper EN ISO 2160 Corr. degree 1 Class 1
Acid index EN 14104 mg KOH/g 0.147 <0.5
Methanol content EN 14110 % m/m 0.003 <0.2
Free glycerol EN 14105 % m/m 0.005 <0.02
Monoglycerids EN 14105 % m/m 0.10 <0.8
Diglycerids EN 14105 % m/m 0.04 <0.2
Triglycerids EN 14105 % m/m <0.01 <0.2
Total glycerol EN 14105 % m/m 0.04 <0.25
Iodine number EN 14111 g Iodine/100 g 100 <120
Phosphorous content EN 14107 mg/kg <1 <4
Alkali content EN 14109 mg/kg <1 <5
 M. Pilar Dorado et al. / Fuel 90 (2011) 2321–2325 2323

ments to correct the Scatter effect [23]. The aim of the use of deriv-
ative spectra instead of raw optical data to perform calibration is to
solve those problems associated with overlapping peaks and base-
line correction [24]. To correlate spectral information of the sam-
ples, and both methanol and glycerol contents, modified partial
least-squares (MPLS) was used as regression method, by using
wavelengths from 400 to 2500 nm every 2 nm. This regression
method reduces the huge number of spectral data points and elim-
inates the intercorrelation of the absorbance values presented by
neighboring wavelengths [25].
Equations were validated by means of cross-validation. Cross-
validation is based on an iterative algorithm, which selects part
of the sample set population to develop the calibration equation.
And then, it uses this equation to predict the content of both meth-
anol and glycerol on the remaining unselected samples. This pro-
cess is repeated until all samples are predicted. The standard
error of cross-validation (SECV) is calculated as the square root of
the mean square of the residuals, considering N-1 degrees of free-
dom and where the residual equals the actual value minus the pre-
dicted one.
The accuracy of the developed calibration models were deter-
mined on the basis of the ratio of performance to deviation
(RPD), statistic calculated as the ratio of the standard deviation
(SD) of the methanol and glycerol values to the standard error of
prediction found in the cross-validation step (SECV) [26], as well
as the coefficient of determination in the cross-validation (r2).
The RPD statistic is considered a useful indicator to evaluate the
prediction capability of an equation to predict the component of
interest. The higher the RPD value, the greater the probability of
the model to predict accurately new samples was found. If the
RPD is >3, the calibration models are considered acceptable for
analytical purposes [26,27].
on the amount of methanol in the sample. This finding indicates it
may be of interest to evaluate results not only from visible together
with NIR region (400–2500 nm), but also from the visible region
only (400–780 nm), provided the easiness and cost saving of the
instruments that work in this spectral range. For this purpose, cal-
ibration equations were built considering methanol content data
and each specific region, thus helping to evaluate the influence of
the spectral region on the prediction capability.
Table 2 gives the calibration statistics values considering differ-
ent spectral regions to predict methanol content in biodiesel sam-
ples. As can be seen, the coefficients of determination (r2) are very
high and reach values close to 1 (0.99 and 0.98 for equations devel-
oped considering visible plus NIR regions, and only visible region,
respectively). The high values of the coefficients of determination
in the cross-validation step indicate calibration models are able
to explain more than 98% of the variability of the reference data.
According to Shenk and Westerhaus [28], r2 values higher than
0.95 show an excellent predictive ability. The SECV value for the
equation to predict methanol content by using the visible plus
NIR spectra is 0.013% m/m with a RPD value of 10.0. Slightly less
accurate statistical results were obtained considering only the vis-
ible region (0.020% m/m for SECV and 6.5 for RPD statistic). How-
ever, in both cases statistics indicate that equations to determine
methanol content in biodiesel samples exhibit high prediction abil-
ity, considering different spectral range [26,27].
Fig. 2 presents the relationship between reference and NIR pre-
dicted values obtained from the equation to predict methanol con-
tent in biodiesel samples, using visible plus NIR spectral data. This
figure confirms the excellent correlation between experimental
and predicted data provided by the NIR calibration model.
3.2. Glycerol contamination

Fig. 4 shows the average and SD spectra obtained from biodiesel

3. Results and discussion
samples contaminated with glycerol, considering visible and NIR

3.1. Methanol contamination

Table 2
Fig. 1 shows the average and SD spectra from biodiesel samples Equations to predict methanol and glycerol presence in biodiesel samples according
contaminated with methanol, obtained by transflectance mode on to different spectral ranges (Standard deviation, SD; standard error of prediction in
cross-validation, SECV; ratio of performance to deviation, RPD).
the visible and NIR regions. As can be seen, average spectra show
NIR absorption bands corresponding to the –CH, –CO and –CC Spectral rangea Mean SD SECV rb RPD
groups (around 1720, 1750, 2150, 2300 and 2360 nm). In the Methanol (%) Visible + NIR 0.222 0.130 0.013 0.99 10.0
visible region (400–780 nm), the spectrum shows maximum Visible 0.222 0.130 0.020 0.98 6.5
absorption at 440 nm, caused by the yellowish color of the sample. Glycerol (%) Visible + NIR 0.030 0.015 0.007 0.75 2.1
Visible 0.030 0.015 0.006 0.81 2.5
Moreover, SD spectrum indicates regions exhibiting higher
a
differences among all biodiesel samples. The main spectral differ- Visible + NIR: 400–2500 nm.
b
ences are observed around the absorption bands at 440, 1720, Visible: 400–780 nm.

1750, 2150, 2300 and 2360 nm, but also around 590 nm (visible re-
gion). At this wavelength, associated to the yellow or orange color
0.5
of the sample, any spectral absorption band (only a shoulder) is
found. Although, different log(1/R) values are depicted, depending y = 1.0079x - 0.0016
0.4
2
R = 0.989

0.3
1 Mean SD 0.006
0.005 0.2
0.8
0.004
0.6 0.1
0.003
0.4
0.002
0.2 0
0.001 0 0.1 0.2 0.3 0.4 0.5
0 0 NIRS predicted values (% Methanol m/m)
400 700 1000 1300 1600 1900 2200 2500
Wavelenghts (nm) Fig. 2. Scatter plot of both experimental and NIR predicted values considering the
best equation for the estimation of methanol in biodiesel samples (visible + NIR
Fig. 1. Average and SD spectra of biodiesel samples contaminated with methanol. range).
2324
regions. The average spectrum is similar to the one produced when
biodiesel was contaminated with methanol (Fig. 1), comprising NIR
absorption bands at around 1720, 1750, 2150, 2300, 2360 nm
(which correspond to –CH, –CO and –CC groups) and 440 nm (re-
lated to the color of the samples). The absence of visually percep-
tible differences in absorption bands may be attributed to the low
concentration of contaminants in biodiesel samples.
Fig. 3 depicts SD spectrum including the spectral regions show-
ing higher differences among biodiesel samples adulterated with
glycerol. Main spectral differences may be found in the region of
1720, 1750, 2150, 2300 and 2360 nm due to different content of
–CH, –CO and –CC groups in each contaminated sample. In the vis-
ible region of the spectrum, the evidence of differences according
to the presence of methanol are displayed at 450 nm (this wave-
length is associated to the blue color).
Table 2 provides calibration statistics values to predict glycerol
content on biodiesel samples, considering different spectral re-
gions. These equations show r2 values of 0.75 and 0.81, considering
visible plus NIR and only visible regions, respectively. It means that
above 75% of the optical data variability may be explained by these
calibration models. In fact, according to Shenk and Westerhaus
[28], r2 values higher than 0.70 show a good predictive ability.
The SECV value for the equation used to predict glycerol content
by using the visible plus NIR spectra is 0.007% m/m, with a RPD va-
lue of 2.1. Statistical results slightly improve when only the visible
region is taken into consideration (0.006% m/m for SECV and 2.5 for
RPD statistic). In this sense, according to Williams and Sobering
[26], calibration models with a RPD value between 2 and 3 indicate
approximate quantitative predictions. As may be seen from statis-
tics included in Table 2, calibration models developed on the basis
of visible and NIR regions to determine glycerol content in biodie-
sel samples present acceptable prediction ability.
Fig. 4 presents the correlation between reference and NIR
predicted values obtained from the equation developed to predict
1 Mean SD
0.8
0.6
0.4
0.2
0 0
400 700 1000 1300 1600 1900
Wavelenghts (nm)
Fig. 3. Average and Standard Deviation (SD) spectra of biodiesel samples contam-
inated with glycerol.
0.06
0.05
y = 1.0486x - 0.0015
2 oil methyl ester as a fuel in a diesel engine. Energy Fuels 2003;17:1560–5.
0.04 R = 0.8097
0.03
0.02
0.01
0.00
0 0.01 0.02 0.03 0.04
NIRS predicted values (% Glycerol m/m)
Fig. 4. Scatter plot of both experimental and NIR predicted values considering the
best equation for the estimation of glycerol in biodiesel samples (visible range).
M. Pilar Dorado et al. / Fuel 90 (2011) 2321–2325
glycerol content in biodiesel samples, using visible spectral data.
As may be seen, predicted data fit experimental ones with a corre-
lation of almost 1:1. However, it exhibits a wider data dispersion,
and thus a lower prediction capability, compared to the model
developed for methanol traces prediction (Fig. 2).
According to our results it is not possible to evaluate the repro-
ducibility. However, the best statistic to estimate the repeatability
of the NIRS calibration equations is SECV. SECV value is calculated
as the standard error of the difference between NIRS predicted and
reference values during the cross-validation step. Thus, it can be
used as a measure of the standard deviation of the repeatability
for the NIRS analytical method. According to the ISO 5725-2 stan-
dard (Accuracy- trueness and precision- of measurement methods
and results) and the values included in Table 2, the root standard
deviation of residual, RSDr (%), for the NIRS prediction of methanol
and glycerol traces could be around 6% and 20% respectively.
4. Conclusions
As a result of the calibration process, the equation with the high-
est prediction ability is able to determine methanol and glycerol
traces in biodiesel samples. The validation set must be provided
with sufficient accuracy to identify those samples. Visible region
analysis also shows significant differences due to the presence of
different contaminants and concentrations. The interesting correla-
tion between color and presence of some contaminants in visible
region may be used as an economical method to assess biodiesel
quality. Moreover, visible and NIRS regions offer an important sav-
ing of time (2 min/analysis) and cost of analysis compared with
other standard reference analysis. From the NIRS calibration and
validation results shown in this work, it can be concluded that
NIR and visible Spectroscopy are able to predict methanol and glyc-
erol traces in biodiesel samples. However, further work is still
needed to improve the calibration statistics for the estimation of
0.01 glycerol content on biodiesel samples.
0.008
Acknowledgments
0.006
0.004 The authors thank to Gloria Fernandez Marin (IAS-CSIC) for
0.002 her support in the lab and to Miquel Vila (Stocks del Vallès, S.A.
‘‘BDP – BioDiesel Peninsular’’) for providing us with biodiesel sam-
ples and analytical analysis to determine biofuel specifications.
2200 2500
This work was funded by Junta de Andalucia, Spain (TEP 4994)
and Ministry of Science and Education, Spain (ENE2007-65490/
ALT).
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