Palm Oil Product Quality Determination

Sponsored Content by Metrohm AGFeb 14 2019

A number of vital parameters of palm oil quality, including Free Fatty Acid
content (FFA), Iodine Value (IV), moisture content, Deterioration of
Bleachability Index (DOBI), and carotene content, were calculated using
Vis-near-infrared (NIR) spectroscopy. This analysis demonstrates how
Vis-NIR spectroscopy can precisely determine these parameters in
concurrent processes.

Introduction
Palm oil is an edible vegetable oil, produced in specific geographic regions,
which is extracted from the fruit of the oil palms and subsequently, distributed
globally for use as an additive in biofuels, or as an ingredient in a broad
spectrum of other products, including cosmetics, cleaning products, processed
food, detergents and shampoos.

Palm oilʼs quality is dependent on the quality of its source material and
preprocessing, and distinctions are made between differing varieties. Crude
Palm Oil (CPO) is derived from the fruit of the palm, while Crude Palm Kernel Oil
(CPKO) is taken from the seed of the trees.

The method of production entails a preprocessing step, followed by a refining

step of CPO or CPKO, during which any scent and color are eliminated. This
refined product, known as Refined, Bleached and Deodorized (RBD) palm or
palm kernel oil, can be divided through additional production stages into a
variety of products, such as RDB olein or RBD stearin.

Each of the products stated has distinct chemical and physical properties,
detailed in various norms and standards, such as Malaysian Standards MS 814
to MS 816. [1–3] Characteristic quality parameters it is necessary to determine
are:

Free Fatty Acid (FFA) Content

The FFA content is a major quality factor of oils and fats. FFAs lack stability
when compared to natural oil and are inclined to oxidize somewhat easily. As
such, this parameter affects shelf life, storage conditions and further
processing. Titration is the usual method employed to determine the FFA
content.

Moisture Content

The shelf life of fats and oils is also indirectly affected by water, which leads to
autocatalytic hydrolysis of oil, resulting in a higher FFA content. Additionally,
bacterial activity can also result from high water content. The standard method
for measuring water content is Karl Fischer titration.

Iodine Value (V)

This is correlated with the quantity of double bonds and offers insight into the
degree of unsaturation of oil. Titration is the standard method for determining
this parameter.

Deterioration of Bleachability Index (DOB)

This parameter determines the complexity of refining crude palm oil and is
dependent on the quality of the palm oil fruits. It is frequently measured using
UV/Vis spectroscopy.

Carotene Content

Carotene is the cause of the reddish color in palm oil, and originates in the
stems of the palm oil fruits. The carotene content is typically determined by
UV/Vis spectroscopy.

Vis-NIR spectroscopy offers an alternate method for quality control of palm oil
products. As will be shown in this article, this analytical method enables each of
the above listed quality parameters to be determined in under 60 seconds,
using concurrent processes.

Configuration
961 samples of CPO, 345 samples of CPKO, 320 samples of RBD olein, and 320
samples of RBD stearin were employed in this analysis. The NIRS XDS Vial
Heater was used at 60 °C to preheat each sample and transform it to a liquid
state.

Samples were analyzed in 8 mm disposable glass in transmission mode on a

Metrohm NIRS XDS RapidLiquid Analyzer over the full Vis-NIR wavelength range
of 400–2500 nm. To circumvent the risk of solidification, the temperature was
maintained at 60 °C.

For data acquisition and management, as well as the development of the

qualification and quantification methods (Fig. 1 and Tab. 1), the software
package Vision Air 2.0 Complete was employed.

Figure 1. A NIRS XDS RapidLiquid Analyzer was used to collect the spectral
data of samples in transmission mode covering the full Vis-NIR wavelength
range of 400–2500 nm.

Table 1. Equipment and software used

Equipment Metrohm code

NIRS XDS RapidLiquid Analyzer 2.921.1410

NIRS 8 mm disposable glass vials 6.7402.000

Vision Air 2.0 Complete 6.6072.208

NIRS XDS Vial Heater 2.9219.010

Results
The ranges of the quality parameters varied across the products tested. For
example, RBD olein samples with an IV between 56 and 59.1 were outside the
calibration range for IV in RBD stearin, which has IV range between 27.8 and
45.1. As such, specific models were created for each product.

These product-specific calibration models can be joined to create a single two-

part operating process. The initial stage, an identity test, is a qualitative model,
which detects the current product (CPKO, CPO, RBD olein or stearin). The
secondary stage is where the software automatically applies the particular
calibration model for the detected class.

Qualitative Analysis

With the NIRS RapidLiquid Analyzer, spectral data can be collected from 400
nm to 2500 nm. As each product displays variations in color (Fig. 2), this
extended spectral range is vital for the application.

Figure 2. Second derivative spectra of different palm oil products in the

spectral range between 400 and 600 nm. The observed strong difference in
intensity is caused by the different color of analyzed samples.

Consequently, qualitative models were created using the entire spectral region,
with second derivative pretreatment and maximum distance in wavelength
space algorithm. Lastly, the library was authenticated in Vision Air Complete
software.

Fig. 3 shows the results of the qualitative analysis, and makes plain that the
ratio of misidentification is negligible and thus, the model is appropriate for the
identification of CPO, CPKO, RBD olein or RBD stearin.

Figure 3. Results of qualitative analysis. The ratio for misidentification is close

to zero.

Quantitative Analysis

The Partial Least Squares Regression (PLS) algorithm in Vision Air Complete
was used to develop the quantification methods for the individual parameters
and products. Depending on which pretreatment brought about the best
analytical figures of merit, the data was pretreated using first or second
derivatives.

Lastly, qualitative and quantitative models were joined in Vision Air Manager to
form a clear and simple-to-use operating process for day-to-day analysis of
varied palm oil products. The correlation plots are exemplarily displayed in Fig.
4–8. These plots show strong correlation between the values identified by the
reference analytical method (x-axis) and the values projected by Vis-NIR
spectroscopy (y-axis).

Figure 4. Correlation plot of reference values from titration versus predicted

values from Vis-NIR for the analysis of FFA in CPO. The FFA content varies
between 2 and 7%.

Figure 5. Correlation plot of reference values from titration versus predicted

values from Vis-NIR for the analysis of moisture in RBD olein. The moisture
content varies between 0 and 0.1%.

Figure 6. Correlation plot of reference values from titration versus predicted

values from Vis-NIR for the analysis of iodine value in CPO. The IV varies
between 30 and 39 mg/100 g sample.

Figure 7. Correlation plot of reference values from UV/Vis spectroscopy versus

predicted values from Vis-NIR for the analysis of carotene in CPO. The carotene
content varies between 400 and 700 ppm.

Figure 8. Correlation plot of reference values from UV/Vis spectroscopy versus

predicted values from Vis-NIR for the analysis of DOBI in CPO. The DOBI varies
between 2.1 and 2.8.

The analytical figures of merit for various palm oil products ratify the strong
correlation results (see Tab. 2–5).

Table 2. Analytical figures of merit for CPKO analysis

Product Range R² SEC SECV

FFA in % 1–5 0.975 0.11 0.12

IV in mg/100 g 18–19 0.535 0.14 0.14

Moisture in % 0.1–0.21 0.495 0.017 0.018

Table 3. Analytical figures of merit for CPO analysis

Product Range R² SEC SECV

FFA in % 2–7 0.878 0.22 0.23

IV in mg/100 g 50–54 0.736 0.33 0.35

Moisture in % 0.06–0.56 0.682 0.045 0.047

Carotene in ppm 416–680 0.709 22.8 23.4

DOBI 2.1–2.8 0.435 0.11 0.12

Table 4. Analytical figures of merit for RBD olein analysis

Product Range R² SEC SECV

FFA in % 0–0.2 0.734 0.012 0.013

IV in mg/100 g 56–57.5 0.726 0.14 0.16

Moisture in % 0–0.1 0.849 0.005 0.006

Table 5. Analytical figures of merit for RBD stearin analysis

Product Range R² SEC SECV

FFA in % 0–0.3 0.931 0.015 0.016

IV in mg/100 g 30–39 0.909 0.58 0.60

Moisture in % 0–0.1 0.683 0.0025 0.0028

Conclusion
A Metrohm NIRS XDS RapidLiquid Analyzer was employed for quality control of
a variety of palm oil products. Results demonstrating low standard errors and
high accuracy were delivered through the calibration models of the Vis-NIR
method.

Vis-NIR spectroscopy has been demonstrated to be a time-efficient technique

for identification and quality control of CPO, CPKO, as well as RBD stearin and
olein. Used alongside the intuitive Vision Air Software, this technique saves on
time and costs during day-to-day analysis of palm oil products.

Additional Information

All results displayed in this article have been used in combination with the data
from other comparable applications to assist in the development of
precalibration for palm oil analysis.

References
h. Malaysian Standard, MS 814 Palm Oil – Specification.
i. Malaysian Standard, MS 815 Palm Stearin – Specification.
j. Malaysian Standard, MS 816 Palm Olein – Specification.

About Metrohm

At Metrohm is one of the worldʼs most trusted manufacturers of high-precision

instruments for chemical analysis. Metrohm was founded in 1943 by engineer
Bertold Suhner in Herisau, Switzerland. Today, Metrohm is represented in 120
countries by subsidiaries and exclusive distributors. The global Metrohm Group
also includes the Dutch companies Metrohm Applikon and Metrohm Autolab,
manufacturers of online analyzers and instruments for electrochemical
research, respectively. Recently, the Metrohm Group was joined by Metrohm
Raman, a leading manufacturer of handheld Raman spectrometers.

Metrohm is the global market leader in analytical instruments for titration.

Instruments for ion chromatography, voltammetry, conductivity, and stability
measurement make the Metrohm portfolio for ion analysis complete.
Instruments for Near-infrared and Raman spectroscopy are another, strongly
growing segment of the Metrohm portfolio.

Metrohm is a problem solver, both in the laboratory and within the industrial
process. To this end, the company offers their customers complete solutions,
including dedicated analytical instrumentation as well as comprehensive
application know-how. More than 30% of the companyʼs employees at the
Metrohm international headquarters in Herisau work in R&D.

Metrohm has been owned 100% by the non-profit Metrohm Foundation since
1982. The Metrohm Foundation, which does not exert any influence on the
companyʼs business operations, sponsors gifted students in the natural
sciences, supports charitable and philanthropic purposes and, above all,
ensures the independence of the company.

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Last updated: Apr 2, 2019 at 9m53 AM