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Methods of Spectroscopy for Selenium Determination: A Review

Article  in  Research Journal of Pharmacy and Technology · December 2019

DOI: 10.5958/0974-360X.2019.01068.0

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 Research J. Pharm. and Tech. 12(12): December 2019

ISSN 0974-3618 (Print) www.rjptonline.org

0974-360X (Online)

REVIEW ARTICLE

Methods of Spectroscopy for Selenium Determination: A Review

Wissam Zam1, Mohamad Alshahneh2, Azez Hasan2
1
Department of Analytical and Food Chemistry, Faculty of Pharmacy, Al-Andalus University for Medical
Sciences, Tartous, Syrian Arab Republic.
2
Department of Analytical Chemistry, Faculty of Science, Tishreen University, Syrian Arab Republic.
*Corresponding Author E-mail: ws.sarah2005@gmail.com, w.zam@au.edu.sy
ABSTRACT:
Selenium (Se) is cumulative nonmetallic element that occurs naturally in a range of oxidation states as volatile
species or analogues of organic sulphur compounds. At low concentrations, selenium is an essential element;
however at higher concentrations it possesses toxicological properties. Its determination requires a sampling
procedure to be followed, an initial digestion stage of the sample matrix and the reduction of Se (VI) to Se (IV).
Spectroscopic methods for the determination of Se including hydride generation atomic fluorescence
spectrometry, hydride generation, graphite furnace, flame atomic absorption spectrometry and
spectrophotometric methods are described detailing detection limits and sensitivity.
KEYWORDS: Selenium; spectroscopic methods; review; detection limits; sensitivity.

INTRODUCTION: Methods of spectroscopy for selenium determination

Selenium is a cumulative nonmetallic element found in Visible absorption spectroscopy:
high concentrations in food and water. It has received A wide number of rapid, highly sensitive and selective
high attention of researchers because of its dual role as spectrophotometric methods for the determination
an essential trace nutrient and a toxic element [1,2]. This selenium (IV) were reported. These methods are based
dual effect has been recognized for many naturally on piazselenol complex formation between the reagents
occurring chemicals[1]. Selenium speciation has been and selenium. Selenium was detected in blood samples
attracting much attention in recent years because based on the oxidation of phenylhydrazine –p sulphonic
selenium compounds have been reported to have acid coupled with acetyl acetone in an alkaline medium
anticarcinogenic activity and prevent heavy metal toxic with a detection limit of 0.07μg/ml[16]. 5,6-diaminouracil
effects[3-5]. Selenium is extensively used not only in hydrochloride reagent was developed and used for the
medicine but also in other fields such as material determination of Se (IV). The reagent formed a yellow
sciences and in the agronomical area[6]. Since that time complex with the aqueous solutions of selenium in acidic
many papers appeared devoted to determination of medium with a detection limit of 0.05μg/ml[17].
selenium in the environment and biological material. The Krishnaiah et al. developed a rapid and sensitive method
most common spectroscopic methods used for for the determination of selenium in environmental
determination of various species of selenium were samples based on either the oxidation of 2,4-
hydride generation atomic fluorescence spectrometry[7,8], dinitrophenyl hydrazine hydrochloride by selenium in
hydride generation [9,10], graphite furnace[11-13] and flame HCl medium and coupling with N-(1-naphthyl)
atomic absorption spectrometry[14,15]. In spite of some of ethylenediamine dihydrochloride with a maximum
the above methods, spectrophotometric methods are absorption peak at 520nm or the oxidation of 4-
popular because of their simplicity and are based on aminoresorcinol hydrochloride by selenium in H2SO4
complex formation between the reagents and selenium. medium and coupling with 4-aminoresorcinol
In view of the profound recent interest in selenium and hydrochloride to yield a orange red colored product with
its vital biological importance in human health, a maximum absorption peak at 495nm. The detection
reviewing modern spectroscopy methods of limits reported were 0.0165 and 0.0335μg/ml,
determination of this element seemed worthwhile. respectively[18]. A similar detection limit of 0.0124μg/ml
resulted from the reaction of selenite ions with
Received on 22.05.2019 Modified on 28.06.2019 hydroxylamine hydrochloride, which in turn diazotizes
Accepted on 24.07.2019 © RJPT All right reserved
Research J. Pharm. and Tech. 2019; 12(12): 6149-6152.
p-Nitroaniline and then coupled with N-1-naphthyl-
DOI: 10.5958/0974-360X.2019.01068.0 ethylenediamine dihydrochloride to form a red colored

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 Research J. Pharm. and Tech. 12(12): December 2019

[10]
azo compound with a maximum absorption peak at 545 . Finally, in order to achieve higher sensitivity in
nm[19]. Soruraddin et al. recently developed a new hydride generation of selenium, sodium tetrahydroborate
spectrophotometric method for the determination of trace (III) (NaBH4) is used as the most suitable reductant for
amounts of selenium (IV) after pre-concentration with hydride generation because of its short reaction time
cloud point extraction. The colored complex was formed coupled with a rapid transfer of the products to the gas
using dithizone at pH < 1 in micellar medium (Triton X- phase. At first, NaBH4 pellets were favorites, but
100) and extracted to a surfactant rich phase by currently more concentrated NaBH4 dissolved in
centrifugation. The proposed method was highly concentrated NaOH or KOH is the most popular and
sensitive with a detection limit of 0.0044μg/ml[20]. most convenient agent[30]. The metal hydride was then
introduced to the atomizer of AAS by inert carrier gas
Hydride generation atomic absorption spectrometer (N2, He) and absorbance is recorded and plotted against
(HG-AAS): concentration[25]. Several operational parameters should
Over the last decade, significant instrumental and be optimized as they could influence the sensitivity of
methodological progress has led to HG-AAS being the HG-AAS method such as the system design and
widely applied to an extensive range of metal sample operating conditions, the type and amount of the acid,
types such as As, Sb and Se which are vaporized by the amount of sodium borohydride, and the generation
converting them into volatile hydrides[21,22]. This method temperature. The sensitivity of this method for selenium
of analysis is one of the most preferred methods because determination ranged from 10.6μg/l to 0.0035μg/l with
of its simplicity, sensitivity and rapidity[23]. Nevertheless, the best detection limit of 0.0055ng/l found by Busheina
the first step of this procedure is the mineralization of et al. who used a HGAAS method for the determination
any organic selenium compound and the reduction of Se of Selenium content in soil samples, alfalfa, animal feed,
(VI) to Se (IV) prior to hydride generation[10]. Different and water samples[25,30,31].
methods have been suggested to accomplish this step
including digestion of the sample using a mixture of a Hydride generation atomic fluorescence spectrometry
wide number of mineral acids such as HNO3, HCL, (HG-AFS):
H2SO4, HClO and H2O2[24]. Several parameters such as Atomic fluorescence spectrometry has been widely used
the type of acid, its concentration and the reaction in single- and multi-elemental determinations since 1964
temperature and time should be optimized to assume a due to its flexibility with a wide variety of light sources,
complete destruction of the organic compounds for optical designs, atomizers, and electronics[32]. Tsujii and
better recovery. Heating the acidified sample greatly Kuga appear to be the first to report the use of non-
enhanced the reduction of Se (VI) to Se (IV) but dispersive AFS for the hydride forming elements such as
unfortunately a wide number of interfering species could As, Sb, Se and Te[33,34]. This approach offers several
be formed[25]. Thus, the reduction of Se (VI) is currently advantages due to the heating process necessary to
carried out using L-cysteine 0.5% at 100ºC for 25 min convert the metal hydride into an atomic vapor[35].
[26]
. The use of solid reagents was also investigated by
Maleki et al. as a simple and fast procedure that could Lopes dos Santos et al. evaluated several conditions for
reduce the interference effects[9]. The effects of several the measurement of the total selenium content in oysters
solid acids such as oxalic, tartaric, adipic, salicylic and using HG AFS after digesting by HNO3 and HCl. Under
some amino acids were evaluated and results proved that the optimized conditions, the detection and the
tartaric acid gave the highest sensitivity. It was also quantification limits were 6.06 and 21.21μg/1,
proved that the increase of solid reagent and the use of respectively[36]. Stibilj et al. developed a method for very
higher volumes of selenium solution improved the lowlevel selenium determination in water soluble protein
sensitivity[27]. However, acid-resistant organoselenium and peptide fractions. The sample was treated using
compounds and high fat samples demand the use of HNO3 and H2O2 and detected by HG-AFS after various
agents with high oxidation potential for complete separation procedures. The LOD was 0.2 μg/l[37]. A new
destruction. Furthermore, selenium readily forms volatile method was proposed for simultaneous determination of
species that could be lost during an uncontrolled traces of arsenic (As) and selenium (Se) in biological
decomposition[28]. The use of a closed microwave samples by HG-AFS from tartaric acid media. The
digestion system was developed as fast procedure that detection limits for arsenic and selenium were 0.13 and
has the advantage to minimize the potential loss of 0.12μg/l, respectively[38].
analyte due to an open system mineralization[29]. Shalt
out et al. proved that the use of microwave-assisted Flame atomic absorption spectrometry (FAAS):
digestion with nitric acid and hydrogen peroxide was Flame atomic absorption spectrometry (FAAS) is one of
appropriate for the complete mineralization of organo- the techniques most extensively used for determining
selenium compounds, avoiding the use of more various elements with a significant precision and
hazardous reagents, such as sulfuric or perchloric acid accuracy. This analytical technique is remarkable for its

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selectivity, speed and low operation cost[39]. It is based of determination was 0.02μg/g[49]. Selenium was
on the light absorption process that passes through the measured in chicken meat either by HG-AAS or by GF-
atomized analyte. The most important stage in the FAAS AAS. Acid digestions were carried out with mixtures of
is the method of atomization of the element that is HNO3 and HClO4. The limits of detection for HG-AAS
analyzed into neutral atoms in the form of gases[40]. and GF-AAS were 1μg/l and 0.6μg/l, respectively [50].
Mariam et al. proposed a method based on the separation
and determination of selenium (IV) ion using CONCLUSION:
polyurethane foam as a solid sorbent coated with A wide number of rapid, highly sensitive and selective
ammonium pyrrolidine dithiocarbamate (APDC). The spectrophotometric methods for the determination
sample was digested by HNO3 and the detection limit for selenium (IV) were reported. However, comparative
this method was 0.064mg/l[41]. Another method was studies have shown that in the past decade atomic
improved in atomic flame absorption spectroscopy to absorption spectroscopy has been established as an
determine the concentrations of AS and Se. Results of adequate method for the determination of selenium in the
the method showed that FAAS is more sensitive to Se sub-ng/ml range. The choice of a particular method will
with an LOD of 1.0mg/l[15]. FAAS is found to be suitable depend on the type of sample studied, accessible
for the measurement of a limited range of elements equipment and analytical experience of the analyst.
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