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A Review:
Analytical methods for heavy metals determination in Environment and human =
samples
Mojtaba
Arjomandib,c and Hamid Shirkhanlood,
bDepa=
rtment
of Water Sciences and Engineering, Science and Research Branch, Islamic Azad
University, Tehran, Iran / Research Institute of Petroleum Industry (RIPI),
Tehran, Iran
c Department =
of
Geophysics, Geological Survey and Mineral Explorations of Iran (GSI),Tehran,
Iran
d,=
sup>à Research Institute of Petroleum Industry, West Entra=
nce
Blvd., Olympic Village, P.O. Box: 14857-33111, Tehran, Iran.
Email of corresponding author: Hamidshirkh=
anloo@yahoo.ca
mustafa.tuzen@gop.edu.tr
Abstract
Heavy metals are vital and necessary in our da=
ily
lives. Moreover, if the amounts of heavy metals are more than the acceptable
amounts (mentioned by WHO) in soil, water, and air, indeed, they cause a lo=
t of
diseases in human bodies. Therefore, monitoring and measuring the amounts of
heavy metals which are arduous and difficult are so important. In this revi=
ew
paper, a lot of studies which have been carried out on the determination and
quantification of heavy metals in human bodies, soil, and water are conside=
red.
Moreover, the effect of toxicity of each heavy metal on human health is
assessed. According to WHO, EPA, NIOSH, ACGIH, and clinical chemistry,
determination of heavy metals such as Cd, Pb, Zn, Hg, Cu, Mn is very import=
ant
in human body and Environmental matrixes. For example, the range concentration of heavy
metals in human body such as, cadmium is about 0.3 to 0.98, and for cooper,=
it
is about 0.01 – 1.107 ppm. In addition, most obtained results
demonstrate that the lowest and highest range concentration of heavy metal=
s in
blood of human body has been equal to 0.56–8.78 ppm and 0.08 – 4.67 ppm
respectively. Finally, in this review paper, the approaches of quantificati=
on
of heavy metals using atomic absorption spectrometry, gas
chromatography, inductively coupled plasma=
mass
spectrometry etc. in human bodies, water, and soil are assessed.
=
Keywords: Heavy metals, Toxicity, Biological and Environmental matrix,
Analytical methods, Nanotechnology
1.&n=
bsp;
Introduction
Many different techniques have been applied for
determination of heavy metal in different samples. Atomic absorption
spectrometry (AAS) is a quantitative method of
metals analysis which was suitable for the determination of 70 elements by
three option accessory (flame, furnace, Hydride generation). AAS measures t=
he
concentration of the metals by passing light (wave length emitted) by a rad=
iation
source of a particular element such as Hg, As, Pb and etc. Many metals
determined by electrothermal atomic absorption
spectrometry (ET-AAS)[1-9], flame atomic absorption spectrometry (F-AAS and
FS-AAS)[10-18], atom trapping flame atomic absorption spectrometry (AT-FAAS=
), Hydride
generation atomic absorption spectrometry, Cold
vapor-atomic absorption spectrometry(HG-AAS, CV-AAS)[19, 20] and
fluorescence spectrometry (XRF) [21-24].=
Also, direct current polarography (DCP) [25, 26],
differential pulse polarography (DPP), neutron activation analysis (NAA),
inductively coupled plasma-optical emission spectrometry (ICP OES)[27, 28],
inductively coupled plasma- mass spectrometry (ICP-MS) [29, 30], UV-VIS [31=
], HPLC-inductively coupled plasma-mass sp=
ectrometry(HPLC-ICP-MS)
[32], electrophoresis(EP) [33], Anodic striping voltammetry (AVS)
Cr(VI) [41]. Cr (=
VI)
compounds, once inside the bloodstream, are actively transported into red b=
lood
cells (RBC) via nonspecific anionic channels and then rapidly reduced to Cr=
(III)
which becomes bound to hemoglobin. As
canceroginic effect of Cr (VI) determination of Cr (VI) very important. Als=
o,
in Figure 1, metabolism and formation of DNA damage by CrVI at pH 7.4 are
shown.
=
Fig.
1. Metabolism, and formation of DNA damage by Cr VI at=
pH
7.4.
Determination of trace heavy meta=
ls
in harvested rainwater by ICP-MS was used by Malassa et al in 2018 [96]. I<=
span
style=3D'font-size:12.0pt;line-height:200%;font-family:"Times New Roman","s=
erif";
mso-ascii-theme-font:major-bidi;mso-hansi-theme-font:major-bidi;mso-bidi-th=
eme-font:
major-bidi;letter-spacing:.1pt;background:white'>nductively coupled plasma =
mass
spectrometry (ICP-MS) was used to quantify the content of each trace h=
eavy
metal (Cr, Co, Mn, Ni, Cu, Zn, Mo, Ag, Cd, Bi, and Pb) in a few rainwater
samples. Their results indicated that that the concentrations of Cr, Mn, Ni,
Ag, and Pb are more than the WHO limits in drinking water [96]. Contaminati=
on of
heavy metals in sediments of the Karasu spring in Nigde, Turkey has been investigated by Yalcin and Narin in 2007 [97]. A few
sediment matrixes were collected from contaminant sites along the spring. M=
oreover,
concentrations of heavy metals have been determined by X-ray Fluorescence
Spectrometer [97]. The amount of Co, Cu, As, Sn, Ni, Zn, Ca, Pb, Al, Fe, Ti,
Cr, and Mn contents of the Karasu creek sediments were equal to 18.30–69.00,
12.40–595.0 5.50–345.3, 5.80–15.1, 10.9–64.1, 28.90–103,300, 4.1–356.2,
7.70–37,840, 13,460–109,400, 11,740–62,900, 22.18–59.04, 41.70–369 and
12.09–3,480 mg/kg respectively. Moreover, according to their results, =
the
presence of a contamination in the Karasu creek is obvious. In the case stu=
dy,
all the metal concentrations are more than acceptable limit values. In
addition, in the Karasu creek and the Akkaya dam, eutrophication has been b=
eing
developed. Also, it sounds that the accumulation of heavy metal in the cree=
k is
come from the discharge of mine quarries, domestic, and industrial wastes [=
97].
Separation of arsenic(III) and arsenic(V) by using
2. =
Experimental
Kaipei Qiu used ultrafi=
ne
mesoporous magnetite nanoparticles (UFMNPs) for removal of heavy metals from waters (Scheme 1).
Ultrafine magnetite NPs(UFMNPs, Fe3O4) were synthesized by co-precipitation =
method
and successfully used as adsorbents for the removal of Pb2+, Cd<=
sup>2+,
Cu2+, and Ni2+ ions from contaminated river water. Al=
so,
the adsorption/desorption tests demonstrated that the ultrafine Fe3O4 NPs
were reusable and can be used several times [139].
Scheme
1. SPE method for extraction heavy metals from liquid=
s
Gollavelli et al and Luo et al used Magnetic Graphene and magne=
tic
chitosan/cellulose microspheres for removal of heavy metal from dinking wat=
ers,
waters [140,141]. Mahmoudi ,Chen and Neyaz can be extracted heavy metals fr=
om
different matrix by iron oxide nanoparticles (SPIONs), Fe 3 O 4 @ SiO 2 and functionalized iron oxide nanomater=
ials [142-144].
Tuzen et al showed a novel method based on switchable hydrophilicity
microextraction syringe system (μS-SHS) by electrothermal
atomic absorption spectroscopy (ETAAS). The proposed method was developed f=
or
separation and determination of vanadium in waters by complexing
2-(5-Bromo-2-pyridylazo)-5-diethylaminophenol (5- Br-PADAP). In this study,
LOD, EF, and RSD were achieved 7.5 ng L-1, 120 and 2.91 %,
respectively. In addition, the μS-SHS is consisting of micropipette tip
and syringe system was designed. First, the 10 mL of real sample was placed=
on
beaker and then, 5- Br-PADAP solutions as ligand were used by sucking into
syringe system. Finally, 0.1 mL of
decanoic acid as a hydrophobic eff=
ect
sucked into to solution which was followed by 500 μL of 1.0 mol L-1 Na=
2CO3
solution as a switchable hydrophob=
icity
for the decanoic acid (CH=
323;(CH=
322;)₈<=
span
style=3D'font-size:12.0pt;line-height:200%;font-family:"Times New Roman","s=
erif";
mso-ascii-theme-font:major-bidi;mso-hansi-theme-font:major-bidi;mso-bidi-th=
eme-font:
major-bidi'>COOH) in liquid phase. The surface response methodology was use=
d to
calculate response surface between [pH]/[V of SHS] and [pH]/[V of Na2<=
/sub>CO3]
of the vanadium. The results showed, high recovery based on 112 μL of =
SHS
and 624 μL of Na2CO3 was obtained at pH=3D3.28. =
The
design of experiments (DOE) was used for analyzing data and optimizing by
surface response methodology [102]. Xiaogang Luo et
al explained a novel sorbent for absorption heavy metals from waters. The carboxyl decorated magnetite (Fe3O4) nanopartic=
les
(MN-CA) were obtained by modifying the magnetite surface with citric acid. =
.In this research, the combination of specifically modified magn=
etic
nanoparticles and activated carbon(AC) to cellulose may create new
nanocomposite adsorbents, which possess high adsorption capacity for heavy
metals removal and easy recovery by magnetic field. It could be deduced that
electrostatic attraction between negatively charged magnetic cellulose-based
beads (MCB) samples and positively charged Cu2+, Pb2+, and Zn2+ was the ini=
tial
driving force of heavy metals binding to the adsorption site of the adsorbe=
nts
[145]. Researcher such as Shannon, Luo, Gericke, Karami and Zhao et al work=
ed
for removal heavy metals from water, water Purification, wastewater treatme=
nt
and methyl orange removal by novel technique with different sorbents such a=
s;
activated magnetic cellulose Microspheres, functional cellulose beads,
magnetite nanoparticles,and hierarchical MWCNTs/Fe3O4/PANI magnetic composi=
te [146-150].
For determining the amount of metals in drinking water samples, the Perkin
Elmer Analyst 700 atomic absorption spectrometer was used by Tuzen and Soyl=
ak
in 2006 [101]. A 10 cm long slot-burner head, a lamp and an air-acetylene f=
lame
were applied. In solid phase extraction (SPE) studies, a glass column with =
100
mm high and 10 mm in diameter was applied [101]. The solid phase materials =
such
as Amberlite XAD-1180, Amberlite XAD-4 and Diaion HP-2MG was purchased, and=
they
were prepared with the washing steps as reported previously in literature. =
They
collected the drinking water samples in prewashed (with detergent, doubly
de-ionized distilled water, diluted HNO3 and doubly de-ionized
distilled water, respectively) polyethylene bottles from eight stations in
Tokat and villages around Tokat in July 2004. The samples were obtained from
the water pump directly after the water had run for at least twenty minutes=
. They
filtered the samples by using a Millipore cellulose membrane with a 0.45 µm
pore diameters [101]. After the process of filtration, nitric acid was used=
to
acidify the samples to 1%, and then the samples were stored in 1 L polyethy=
lene
bottles. The samples were thereby stored at 4 °C for a short time, afterwar=
ds
they were analyzed until the changes of the physicochemical form of the met=
als
were minimized [101]. Electroplating industry, tanneries, electronics
manufacturing industry, coal-fired power plants and mining operation are key
sources of heavy metal pollution in water [151]. Lead (Pb) is discharged into water sour=
ces
from various industries and is highly toxic to human beings even at trace
concentrations. Maximum contaminant level of Pb(II) in drinking water is se=
t at
15 μg L−1 by US Environmental Potential Agency (US EPA). Chromiu=
m(Cr),
another toxic heavy metal pollutant, is mainly present in the effluents of
leather tanning, electroplating and chromate preparations. Chromium is foun=
d in
two oxidation states Cr(III,VI) and Cr (VI) is more toxic. World Health
Organization (WHO) guideline for Cr(VI) in drinking water is 50 μg L−1.
So determination and separation this pollutant from waters with novel techn=
ique
based on sorbent adsorption is very important [151]. Santhosh et al showed lead and Cr simpl=
y extracted
from water solutions by PG-C and CNF-C [151]. By using thermal process, cob=
alt
ferrites (CoFe2O4) paste on porous graphene (PG) and
carbon nanofibers (CNF)), which was named PG-C and CNF-C nanocomposites as
magnetic adsorbents [151]. In Figure 2, removal of heavy metals using
nanographene is shown.
Sarika Singh et al used a functional oxide nanomaterials and
nanocomposites for the removal of heavy metals and dyes in liquid phase. Th=
ey
showed that the oxide-based nanomaterials, such as Fe3O4,
ZnO and TiO2 for the removal of different toxic metals and organ=
ic
dyes at optimized pH. Magnetic nanoparticles as excellent sorbent can be us=
ed
as highly effective, efficient and economically-viable for removal toxic me=
tals
with advantages of easy separation under a magnetic field for reuse. Shen e=
t al
have observed that the adsorption efficiency of Ni2+, Cu2+<=
/sup>,
Cd2+ and Cr6+ ions by Fe3O4
nanoparticles is strongly dependent on pH, temperature, and the amount of t=
he
adsorbent. In optimized conditions, 3.5 mg mL-1 dose of
nano-adsorbent with an optimum pH=3D4 was used for removal heavy metals fro=
m contaminated water [152]. Phoebe Zito Ray et al studied on Inorganic nano-adsorbents for =
the
removal of heavy metals and arsenic in aqueous solutions. They were explain=
ed
that metal oxides and CNTs as nanoadsorbents were used for heavy metal remo=
val
in aqueous solutions. Phoebe Zito Ray et al
used the iron oxide (hematite, magnetite and maghemite), carbon
nanotubes (CNT), and metal oxide based (Ti, Zn) and polymeric nanoadsorbents
for this study. Based on reults, metal oxides can have increased surface ar=
ea
and possess favorable sorption to heavy metals. ZnO nanoplates showed compl=
ete
removal of Cu2+ in aqueous solutions [153]. Recently,
CNTs and nZVI synthetized by coupling these nanomaterials and was efficient
used for removal of Cr(VI), Se and Co from polluted water by Giorgio=
Vilardi
et al. Regeneration studies were performed fixing CNTs-nZVI concentration a=
nd
the initial metal concentration equal to 10 mg L-1, as already
reported in a previous study [154]. Experimental
results of adsorption batch tests showed that the removal efficiency of
nanomaterials was in decreasing order: CNTnZVI>nZVI>CNTs>CNTs-nZVI,
except for the Cr(VI) that nZVI was the most efficient material. Furthermor=
e,
the removal of Cr(VI) was found to not be affected by varying the pH in the
case of using nZVI, but decreased with increasing pH when using the other t=
hree
nanomaterials[154]. Also, Majed Alrobaian and Hassan Arida studied on
Assessment of Heavy and Toxic Metals in the Blood and Hair of Saudi Arabia
Smokers Using Modern Analytical Techniques. The levels of some selected heavy and
toxic metals (e.g.; Hg, Pb, Cd, As, Se, Mn, Zn, Ni, and Cr) were determined
using inductively coupled plasma-atomic emission spectrometer (ICP-AES). Pr=
ior
to the analysis, the blood and hair samples of Saudi Arabia smokers were
collected, treated, and digested by microwave digestion system. The validat=
ion
measurement of ICP-AES was performed using working calibration solutions of=
the
investigated toxic heavy metal ions (Hg, Pb, Cd, As, Se, Mn, Zn, Ni, and Cr=
) [155].
Kaiser, Zheng
and Feng was introduced a novel two-dimensional polymers synthesis with nano
size in water which was different application such as heavy metal removal. =
They
reported the controlled synthesis of few-layer two-dimensional polyimide
crystals on the surface of water through reaction between amine and anhydri=
de
monomers, assisted by surfactant monolayers [156]. Heavy metals such a l=
ead
or cadmium has devastating health effects on human body. So, removal of hea=
vy
metals from industrial wastewater and drinking water is very important.
Rosillo-Lopez et al showed that carboxylated graphene nanoflakes (cx-GNF),
, is more than six times greater for the cx-GNF compared to GO which is att=
ributed
to the efficient formation of lead carboxylates as well as strong cation–=
960;
interactions [157]. Zhao et al introduced a novel multi-throughput dynam=
ic
microwave-assisted leaching (MDMAL) combined with ICP-AES was used for the
simultaneous determination of Cu, Mn, Zn and Pb in soil. The MDMAL method w=
as
more rapid than the simple digestion method or microwave digestion process =
and
could be an alternative approach for the analysis of heavy metals in solid
samples [158]. Aaron et al
reported an efficient chemical strategy for the crosslinking of polymer cha=
ins
based on the N- and C- of proteins(CPC→N/C-P), producing hybrid hydro=
gels
which was related to biomolecules. This compound is largely independent of =
the
protein’s sequence; it can in principle be used to incorporate of polypepti=
de
into a polymer based on uniform linkages. They used cysteine for this strat=
egy
to convert metallothioneins into a recyclable polymer gel that can remove h=
eavy
metals from water samples [159]. Shirkhanloo et al reported a novel method based on
amine-functionalized mesoporous silica UVM-7 as nanoadsorbent for manganese (II) and manganese (VII)<=
span
style=3D'mso-spacerun:yes'> extraction in waters by ultrasound
assisted-dispersive-micro-solid phase extraction (US-D-μ-SPE) procedur=
e.
They were used NH2-UVM7 for speciation of Mn(II) and Mn(VII) ions at pH of 8
and 5, respectively which was dete=
rmined
by(AT-F AAS. The validation of the method was also performed by the standard
reference material [160]. Also, Shirkhanloo et al introduced a
carboxyl-functionalized nanoporous graphene (NG-COOH) as solid phase sorbent
for speciation of trace Hg (II) and R-Hg (CH3Hg+ and =
C2H5Hg+)
in waters by US-D-IL- μ-SPE (pH=3D8). Ionic liquid was used for trappi=
ng of
sorbent from water sample. After back extraction, Hg (II) concentration
determined with flow injection-cold vapor-atomic absorption spectrometry
(FI-CV-AAS) [161]. Also they were =
reported
a new method based on ultrasound assisted-dispersive solid-liquid multiple
phase microextraction (USA-DSLMPME) for speciation of trace amounts of
inorganic arsenic (III and V) and total organic arsenic (TOA) in waters and
human urine samples. By procedure NH2-UVM7 were immersed in ionic liquid (I=
L)
as an extraction phase. Then, the mixture of NH2-UVM7 and IL/acetone
[HMIM][PF6]/AC) was injected to sample at pH of 3.5. After ultrasonic, As(V) anion extracted=
by
binding to amine group. Total amount of inorganic arsenic (TIA) was determi=
ned
after oxidization of As(III) to As(V) by ETAAS and As(III) was calculated by the subtracti=
ng TIA
and As(V) content [162]. and nano-graphene oxide (nGO) can be
extracted Fe2+, Cu2+, Fe3+, Cd2+ and
Pb2+ ions from water sample. The sorption capacity for Pb2+
3. Results and Conclusions
Kaipei
Qiu was introduced a novel adsorption process for heavy
metals from waters. In the adsorption process, the desorption and repeatabi=
lity
are significant parameters for developing new adsorbents for practical
applications. The heavy metals such as, Pb2+, Cd2+, C=
u2+,
and Ni2+ were adsorbed by UFMNPs
which was shown in Schem=
e 2. The adsorption kinetics is one of=
the
important characteristics defining the effectiveness of an adsorbent, which
describes the solute uptake rate by controlling the diffusion process and t=
he
residence time of an adsorbate uptake at the solid/solution interface. The
results in this quaternary Pb–Cd–Cu–Ni system indicated that the rate const=
ant
of Pb2+ (0.045 g mg–1 min–1) was
higher than the rate constants of Cu2+ (0.008 g mg–1=
sup> min–1),
Cd2+ (0.005 g mg–1 min–1), and N=
i2+ (0.003
g mg–1 min–1), further demonstrating the strong
affinity of Fe3O4 NPs for Pb2+[139].&=
nbsp;
Scheme 2.
Removal of heavy metal Ions by desorption process [139]
=
Soylak
and Tuzen studied on the amounts of Cr, Cu, Ni, Zn, Mn, Fe, Co, and Al in
drinking water samples based on novel extraction technique using atomic
absorption spectrometry in Turkey. According to their studies, the
concentration of Cr in natural water was often very small. Based on results, the hexavalent form of=
chromium
(Cr VI) is ranged between 3.14 and 6.08 µgL-1. The me=
an
of Cr levels in the waters of the area of Turkey was equal to4.40 µgL-=
1.
Maximum tolerable limit of concentration of total chromium in drinking water
was less than 50 µg/l (Tlv of chromium by WHO > 50 µg L-1) [1=
01].
The permissible value of Ni in drinking water was less than 20 µg L-1<=
/sup>.
The mean level of Ni in the water samples, in the area of Tokat, Turkey was=
equal
to 3.82 µgL-1 which was lower than standard references such as E=
PA,
WHO. Also, according to their stud=
y, the
drinking water sample from Turhal was the highest nickel value (5.35±0.28 µ=
g/
l) and the city center of Tokat was the lowest (2.16±0.19 µgL-1)=
[101].
They showed, the amount of Cu was in the range of 4.44-7.43 µgL-1. In
Erbaa, Turkey, Cu was substantially lower than the permissible limit define=
d by
WHO (1.0 µgL-1) in drinking waters [101]. In addition, mean leve=
l of
concentration of Cu was equal to 6.01 µg L-1. Therefore, no
contamination of Cu was there in the drinking water samples. The guideline
value for zinc in drinking-water is given as 5.0 mg/l by WHO. The concentra=
tion
of Zinc ranged from 4.16 to 8.44 µg L-1 in the drinking water
samples. The mean level of zinc was obtained 6.12 µg L-1, which =
was
more than the permissible limit value (5.0 mg/l) [101]. Many published meth=
ods were
reported for determination and sample preparation of heavy meta=
ls
in water and biological samples [Table 1-3]. Chromium speciation based on
acetylcysteine (NAC) by dispersive liquid–liquid bio-microextraction was
achieved in human blood samples by shirkhanloo et al. By method, Ionic liqu=
id
(1-hexyl-3-methylimidazolium hexafluorophosphate) was rapidly injected into=
the
blood samples containing Cr3+, which have already complexed by N=
AC
at pH from 5 to 8. By optimizing, the linear range, limit of detection and
preconcentration factor were achieved 0.03–4.4 µg L−1, 0.0=
05
µg L−1, and 10 respectively [163,164]. Also, chromium
speciation was reported by other researcher [165-172]. Xiaogang Luo et al explained a novel sorbent for absorption heavy metal=
s from
waters by syntesis of MCB.=
The
carboxyl decorated magnetite (Fe3O4) nanoparticles (MN-CA) were obtained by
postmodifying the magnetite surface with citric acid. The
nanoparticles of Fe3O4 were added to 0.1 M citric acid under ultrasonic
condition for 45 min, and the reaction was kept for 4 h at room temperature=
. A
magnet was used to separate the MN-CA, and then the prepared MN-CA samples =
were
rinsed thoroughly with acetone and double distilled water. The proposed met=
hod
based on MN-CA followed by Scheme 3 for
adsorption heavy metals from waters [145].
Scheme 3. depiction of preparation of =
MCB
and the adsorption mechanism of heavy metal ions by MCB[145].
Naeemullaha et al showed, the effect of main
parameters on extraction of vanadium in waters was evaluated by μS-SHS
procedures [102]. For optimizing,
Statistical assessment of μS-SHS method, Screening and optimization of
experimental variables and selectivity of the μS-SHS method was studied
and finally, the method was validated by CRM (SLRS-4 Riverine water
samples). The optimization of experimental variables followed with screen o=
ut
of the volume of SHS, pH, volume of Na2CO3 and volume=
of
H2SO4 solution as a extraction efficiency with t-value
(95 %) of 2.365. The simple, fast and switchable hydrophilicity microextrac=
tion
(SHM) couple with ETAAS through micropipette tip syringe system (μS-SH=
S)
was used for separation and determination of vanadium in food and water
samples. The μS-SHS method introduced an ideal sample preparation for
vanadium extraction. The simple, fast and applied method based on SHM had g=
ood
efficiency as compared with conventional methods for extraction of vanadium=
[102].
Also, the proposed method based on μS-SHS compared wi=
th
published method and results showed high precision and accuracy results with
low LOD and RSD (Table 1). Moreover, the graphical
abstract of the μS-SHS was shown in Figure 3.
Table 1. the proposed method based on μS-SHS compared wi=
th
published method [102]
|
Sample prepration |
Technique |
SV |
RSD% |
LOD (μg.L-1) |
EF/PF |
References |
|
SPE |
ICP-OES |
10 |
3.4 |
0.06 |
45 |
68 |
|
CPE approach |
Spectrome=
tric |
…. |
…. |
1.4 |
…. |
70 |
|
CPE/ETAAS |
|
50 |
…. |
0.042 |
125 |
71 |
|
|
|
|
|
|
|
|
|
μS-SHS/ETASS |
|
10 |
2.2 |
0.0075 |
120 |
76 |
Fig. 3. The graphical abstract of the μS-SHS=
[102].
Many separation methods were used for determination of ultra-tr=
ace
metals in different matrix, such as Liquid-liquid microextraction, dispersi=
ve
liquid–liquid microextraction, solid-phase
microextraction, selective dispersi=
ve
micro solid-phase extraction, traditional organic solvents, and
switchable solvent, ultrasound
assisted-dispersive-ionic liquid-micro-solid phase extraction and ultrasound
assisted-dispersive solid-liquid multiple phase microextrbased on action =
span>[Table
1- 3]. Kaiser, Zheng and Feng used a novel two-dimensional polym=
ers
crystals (TDPC) synthesis with nano size in waters through reaction between
amine and anhydride monomers by surfactant monolayers. They showed high
crystallinity polymers (CsP) with thickness (2 -3 nm) and an crystal =
size
(3.5 μm2). The molecular structure of the materials, =
were
characterized using X-ray scattering and TEM. The structure and TEM was sho=
wn
in Figure 4. The formation of CsP is attributed to the pre-organization of
monomers at interface phase (water- surfactant). Finally, micrometre-sized =
and
few layer TDPC were grown. This material was used in different application =
such
as removal heavy metals [156].
Fig. 4. The stru=
cturea
and b) TEM of two-dimensional polymers crystals (TDPC)[156]
Rosillo-Lopez et al u=
sed carboxylated
graphene nanoflakes (CX-GNF) and
nanographene oxide (GO) for extracting of heavy metals such as, Fe2+, Cu2+, Fe2+ or
Mg2+ cations which were already existed in environmental
matrix. So, the CX-GNF material showed the highest potential for extraction=
of
heavy-metal from water as compared to other graphene materials [157]. Zhao =
et
al used
Aaron et al, showed that, the crosslinking of polymer chains ba=
sed
on the N- and C- of proteins (CPC→N/C-P) was used as a key of the
proteins which was captured trace amounts of heavy metals such as cadmium in
the presence of innocuous ions in contaminated water sample. Protein-cross-=
linked
hydrogels introduced for sequestration of heavy metal ions in water samples=
. As
figure 7, the Pea metallothioneins (PMTs) can capture toxic metal ions by
condensing to form binding pockets. The synthetic route to access these
materials involves the introduction of ketones on both protein termini. The=
se
groups are then used to cross-link alkoxyamine-substituted polymers through
oxime formation [159]. Shirkhanloo et al=
used NH2-UVM7
based on US-D-μ-SPE method for speciation of manganese in water sample=
s.
The batch adsorption capacity of NH2-UVM7 for Mn(II) =
and
Mn(VII) ions was found to be 1733 μmol g−1 and 570
μmol g−1, respectiv=
ely.
In optimized parameters, LOD (3Sb/m), and LOQ (10Sb/m) were 0.007 μg L=
−1 and 0.03
μg L−1 for Mn(II).
The mean preconcentration factors for Mn(II) and Mn(VII) were calculated as
102.3 and 98.8 with RSD about 2.8%, respectively (Fig. 8). The regression equations for
the calibration curves of Mn(II) and Mn(VII) were A=3D9.8438 C+0.0053
(R2=3D0.9997), and A=3D9.6922 C+0.0045 (R2=3D0.9995), respectively [160]. In
addition, Shirkhanloo et al used NG-COOH f=
or
speciation of trace mercury in waters by US-D-IL- μ-SPE. Under optimiz=
ed
conditions, the linear range, LOD and PF/EF were obtained 0.03–6.3 μg =
L−1, 0.0098
μg L−1and 10.4 for
caprine blood samples, respectively. The developed method was successfully
applied to natural water and human/caprine blood samples. In order to validate the method described, two certif=
ied
standard reference materials, NIST-SRM 995c (mercury species in caprine blo=
od)
and NIST-SRM1641e (total mercury inwater), were analyzed by US-D-IL-
μ-SPE [161]. They used NH2-UVM7 bas=
ed on
USA-DSLMPME for speciation of trace amounts arsenic (III and V) in waters a=
nd
human urine samples. The
linear range, LOQ (3σ<=
/span>), RSD% and EF for As(V)were obtained 0=
.02–1.65
μg L−1, =
11
ng L=
−1, 4.3% and 100.5. The recoveries (95=
span>–102%
) was achieved by certified reference material in urine (NIST-SR=
M). The mean of LOD was obtained 3.3 ng L−1 and 2.7 ng L−1 for human urine and standa=
rd
samples, respectively (intra-day, Mean of LOD =3D 3)[162].
=
Fig.7.=
Pea metallothioneins (PMTs) can capture =
toxic
metal ions a) condensing to form binding pockets b) ketones used to cross-link
alkoxyamine-substituted polymers [159]
=
Fig.
8. Procedure of Mn speciation based on NH2-UVM7=
sub>
by US-D-μ-SPE procedure [160].
3.1.=
Chemistry techniques for heavy
metals
Also, many chemistry techn=
iques
were reported in published papers for separation, extraction, preconcentrat=
ion
and speciation metals in different matrixes (Table 2). Recently, the
liquid-liquid extraction methods (LLE) were used for separation and
determination heavy metals from water and human biological samples. Some of=
LLE
techniques such as, ultrasonic-thermostatic-assisted cloud point extraction
procedure (UTA-CPE-FAAS), aqueous solvent-based dispersive liquid-liquid
microextraction (AS-DLLME), cloud point extraction - slotted quartz tube-fl=
ame
atomic absorption spectrometry (CPE-SQT-FAAS), surfactant-assisted dispersive liquid–liquid
micro-extraction (SA-DLLME-FAAS), s=
witchable
liquid-liquid microextraction (SLLME-SQT-FAAS), surfactant-Based
Dispersive Liquid-Liquid Microextraction based on FAAS(SB-DLLME-FAAS), =
; vortex-assisted DLLME based on
voltammetric (VA-DLLME-VM), =
span>micro=
wave-assisted
extraction - induc=
tively
coupled plasma-optical emission spectrometry (=
MAE-ICP-OES),
Ionic liquid-based microwave-assisted dispersive liquid-liquid microextract=
ion
(IL-based MA-DLLME), Ionic liquid-based dispersive liquid-liquid
microextraction (IL-DLLME), Ionic liquid ultrasound assisted dispersive
liquid-liquid microextraction (IL-UA-DLLME), In-situ ionic liquid
dispersive liquid-liquid microextraction(in-situ IL-DLLME),
microwave-assisted extraction and dispersive liquid–
Table 2. Solvent
extraction for determination and separation of heavy metals in different ma=
trix
[173-197]
|
Sample |
Metals |
Method |
Solvent /Ragent |
EF/PF |
LOD μg L−1 |
Ref. |
|
Wastewater |
Cd |
DLLME/SQT-FAAS |
DPC |
93.3 |
0.5 |
[173] |
|
Milk Vegetables
Foodstuffs |
V(V) and Mo(VI) |
UTA-CPE-FAAS |
Nile blue A - PONPE |
145 and 115 |
0.86 and 1.55 |
[174] |
|
Parsley |
Cd |
CPE-SQT-FAAS |
DPC |
60 |
0.0007 |
[175] |
|
Tap River Well water |
Zn |
SA-DLLME-FAAS |
PAR |
----- |
0.5 |
[176] |
|
Wastewater |
Co |
DLLME/SQT-FAAS |
DPC |
86.56 |
0.97 |
[177] |
|
Tea vitamin B12 |
Co |
SLLME-SQT-FAAS |
Schiff base ligand |
107.7 |
3.1 |
[178] |
|
Food
Water
Samples |
Cu(II) |
SB-DLLME-FAAS |
Triton X-114 |
50 |
1.61 |
[179] |
|
Milk |
Cd(II), Cu(II), Pb(II) |
DLLME/FAAS |
TDES=
span> |
---- |
0.38–0.42 |
[180] |
Chocolate
|
Ni |
PV-IS-DLLME |
APDC |
17 |
100.0 |
[181] |
|
Urine |
Hg |
VA-DLLME-VM |
AuNPS-PE |
--- |
1.1 - 1.3 |
[182] |
|
human
blood |
Cr(III and VI) |
CP-DILLME-ET-AAS |
IICDET |
25.2 |
0.0054 |
[183] |
|
Human
serum |
Cd |
DLLME-ETAAS |
TSILs |
10.2 |
0.005 |
[184] |
|
Human
blood |
Cr(III and VI) |
IL-DLLBME-ETAAS |
NAC |
10 |
0.005 |
[185] |
Biodiesel
|
Na, K, Ca and Mg
|
RP-DLLME/FAAS |
Iisopropanol,HNO3, |
---- |
0.006- 0.026 |
]186] |
|
Water |
Ta (I), Ta (III) |
IL DLLME-ET-AAS |
[C6MIm][PF6] |
100 |
3.3 ng L−1 |
[187] |
|
Cosmetic
|
Hg (II), MeHg+ ,EtHg+ |
HPLC-ICPMS |
[C6MIm][PF6] |
760, 115, 235 |
1.3 ng L−1 |
[188] |
|
Wines |
As (III) |
DLLME-ETAAS |
[C8MIm][PF6] |
---- |
5.0 ng L−1 |
[189] |
|
Water |
Cu(II) |
DLLME-FAAS |
[C4MIm][PF6] or [C16C4Im][Br] |
54 |
3 300 ng L−1 |
[190] |
|
Water
and leaves
|
Rh (III) |
US-IL DLLME-FAAS |
[C8MIm][NTf2] |
---- |
0.37 |
[191] |
|
Water |
V (IV) and V (V) |
TC-IL DLLME-ETAAS |
[C4MIm][PF6] |
---- |
0.0049 |
[192] |
|
Tea,
Soda Beer Milk |
Se (IV) |
USA-IL-DLLME-ETAAS |
[C6MIm][NTf2] |
150 |
12 |
[193] |
|
Water |
Au, Ag |
MRTILs- DLLME-ETAAS |
[C5(MIM) |
245 and 240 |
3.2 and 3.7 |
[194] |
|
Food |
Zn, P, Cd, Pb, Fe, Mn, Mg, Cu, Ca, Al, Na, K |
MAE -ICP-OES |
MAE |
---- |
0.01 mg kg−1 -7.8 mg&=
#8239;kg−1 |
[195] |
|
Water |
Pd and Pt |
CPE-ICP OES |
MBT |
--- |
0.525 and 0.752 |
[196] |
|
Water
serum |
Cu(II) |
IL-mE-DLLME-CPE-ETAAS |
Oxine-IL |
70 |
0.132 |
[197] |
EF: Enrichment Factor
=
=
UTA-CPE-FAAS:
ultrasonic-thermostatic-assisted cloud point extraction procedure
AS-DLLME: Aqueous solvent-based dispersive liquid-liquid
microextraction
DPC: Diphenylcarbazone
Nile blue A:
9-(diethylamino)benzo[a]phenoxazin-5-ylidene]azanium; sulfate-PONPE
(polyoxyethylene-nonylphenyl ether
ETAAS: Electrothermal atomic absorption spectrometry
FAAS: Flame atomic absorption spectrometry
=
=
SQT-FAAS:
Slotted quartz tube-flame atomic absorption spectrometry
=
=
CPE-SQT-FAAS:
Cloud point extraction - slotted quartz tube-flame atomic absorption
spectrometry
=
=
DPC:
Diphenylcarbazone
=
SA-DLLME-FAAS : Surfactant-assisted
dispersive liquid–liquid micro-extraction
=
PAR: 4-(2-pyridylazo) resorcinol
=
SLLME-SQT-FAAS: Switchable liquid-liquid microextraction<=
span
style=3D'mso-spacerun:yes'>
=
=
SB-DLLME-FAAS:
Surfactant-Based Dispersive Liquid-Liquid Microextraction/FAAS =
=
Triton X-114: Surfactant=
=
TDES: Ternary deep eutectic solvent
=
=
APDC:
ammonium<=
/i>=
pyrrolidine
dithiocarbamate
=
=
VA-DLLME-VM:
Vortex-assisted DLLME/ voltamm=
etric
=
=
AuNPS-PE:
gold nanoparticle-modified screen-printed electrodes
=
=
MAE-ICP-OES:
microwave-assist=
ed
extraction - inductively coup=
led
plasma-optical emission spectrometry
=
=
MBT:
2-mercaptobenzothiazole
=
=
Oxime-IL:
8-hydroxyquinoline-IL
UA-DLLME: Ultrasound-assisted dispersive liquid-liquid
microextraction
UAE- IL-DLLME: Ultrasonic-assisted ionic liquid based dispersive
liquid–=
liquid
microextraction
USA-DLLME: Ultrasound-assisted dispersive liquid-liquid
microextraction
USA-IL-DLLME: Ultrasound assisted ionic liquid dispersive
liquid-liquid microextraction
Table 3. Different sorbents for extraction of heavy metals in human a=
nd
environmental samples [198- 218]
|
Sample |
Method |
Sorbent |
Heavy met=
als |
LOD (ng
L−=
span>1) |
EF/PF |
AC(mg g-1) |
Ref. |
|
Serum Blood |
USA-D-µSP=
E-ETAAS |
NH2<=
/sub>-UVM7 |
Cd |
2.0 |
25 |
108.6 |
[198] |
|
Waters |
MCD-µSPE-=
ETAAS |
GSH |
Pb, Cd, C=
r |
8.9, 4.0,=
10 |
17, 18,17=
|
146.3, 13=
2.5,
125.8 |
[199] |
|
Waters River |
USA-CP-MS=
PE |
AFSA |
Pb |
10.0 |
102 |
--- |
[200] |
|
Urine Water |
USA-DSL-M=
PME |
NH2<=
/sub>-UVM7 |
As I=
II,
AsV |
1.1 |
100.5 |
--- |
[201] |
|
Blood Water |
US-D-IL-
µSPE-AT-FAAS |
NG-COOH |
Hg, MHg, =
EHg |
9.8 |
10.4 |
153.7, 12=
5.8,
125.8 |
[202] |
|
Water Tap W |
US-D- µSP=
E |
NH2<=
/sub>-UVM7 |
Mn I=
I
, Mn VII |
7.0, 8.0<= o:p> |
102.3, 98=
.8 |
1733 and 570 µmol.g |
[203] |
|
Serum Blood |
USA-D- µS=
PE |
GONPs |
Al |
20.0 |
25 |
187.5 |
[204] |
|
Water Drinking |
SPE-FAAS<= o:p> |
CdSNPs |
Pb, Cu |
--- |
--- |
200, 166.=
7 |
[205] |
|
Wastewater |
FTIR |
G+MGO |
Pb2+, d2+ ,Cu2+<=
/sup> |
--- |
--- |
358.96, 388.4, 169.8 |
[206] |
|
Waters |
SPE-FAAS<= o:p> |
GO |
Pb, Ni |
1400–2100=
|
95-102.5<= o:p> |
195, 178<= o:p> |
[207] |
|
Waters |
ET-AAS
|
GO-NH2
|
Pb (II) |
9.4 |
100 |
479 |
[208] |
|
serum urine |
H-US-D-μ-SPE |
G-COOH |
As speci=
es |
2.1 |
53 |
125.4 |
[209] |
|
River water |
CHD-μSPE |
GO |
Pb, Cd, C=
r |
110, 15, =
38 |
15 |
---- |
[210] |
|
Waters |
SPE-ETAAS=
|
MnO2=
/
CNT |
PB, Cd |
4.4, 1.5<= o:p> |
100 |
---- |
[211] |
|
Waters Urine |
DμSP=
E-TRXRFS
|
MWCNT |
Cr (=
VI) |
3000 |
66 |
154.3 |
[212] |
|
Soils Waters |
SPE-ICPMS=
|
Ti- MSN |
Cu |
3.9 |
10 |
---- |
[213] |
|
Blood |
M-SPμ=
;E-FAAS |
Modified =
carbon
cloth |
Cd |
150 |
10 |
---- |
[214] |
|
FOOD |
SPE-FAAS<= o:p> |
Dowex
Marathon C |
Pb |
130 |
250 |
---- |
[215] |
|
Agricultur |
SPE-FAAS<= o:p> |
F-MOF |
Zn |
200 |
238 |
---- |
[216] |
|
Foods |
SPE-FAAS<= o:p> |
B2O3/TiO2=
|
Cd |
1440 |
50 |
172.5 |
[217] |
|
Waters |
D-μS=
PE-ETAAS |
NH2<=
/sub>-SiO2-GO |
Pb |
9.4 |
100 |
---- |
[218] |
AC: Absorption Capacity
EF/PF: Enrichment
factor/preconcentration factor
ET-AAS: Electro-thermal at=
omic
absorption spectrometry
FAAS: Flame atomic absorpt=
ion
spectrometry
GSH: Graphene<=
i>-silica hybrid
USA-D-μSPE: Ultrasound
assisted-dispersive-micro solid phase extraction
MCD-μSPE:
Moderate centrifugation-assisted dispersive micro solid phase extraction
USA-CP-MSPE: Ultrasound-assisted cloud
point-micro solid phase extraction
AFSA: Amine functionalized silica aerogel =
USA-DSL-MPME: Ultrasound
assisted-dispersive solid-liquid multiple phase microextraction
US-D-IL-μ-SPE=
: ultrasound assisted-dispersive-ionic liquid-micro-sol=
id
phase extraction
NG: Nanographene
=
CHD-μSPE: Coagulating homogenous dispersiv=
e micro-solid
phase extraction
CdSPNs: Cadmium
Sulfide Nanoparticles
=
TRXRFS: Total reflection X-ray fluoresce=
nce
=
GONPs: Graphene oxide nano-particles
=
M-SPμE: Miniaturized solid phase
microextraction
=
=
SPE-FAAS: Solid phase extraction-flame atomic absorption spec=
trometry
=
GO-NH2:
Aminosilanized graphene oxide
The affinity of Hg towards Au was generally achieved by AuHg,
AuHg3, and Au3Hg [219]. Lisha et al. reported the removal of Hg (II) with
nanoparticles of Au (AuNPs) coated on aluminum [220]. NaBH4 helped to reduc=
e Hg
(II) to Hg (0) and removed by AuNPs with
capacity of 4.0 g g −1. Also, Jiménez et al. was used
citrate-coated AuNPs for extraction mercury in water [221]. Absorption merc=
ury
with AuNPs was shown in Figure 9.
Fig. 9. The absorpt=
ion
mercury by AuNPs
Magnetite (Fe3O4)as nanoadsorbent was used for heavy metal remo=
val
as environmental friendliness. Fe3O4 could be easily separated from liquid
phase. Fe3O4 was used for heavy metals treatment in waters [222-224]. Giral=
do
et al. synthesized magnetite nanoparticles by using a co-precipitation meth=
od
and were used for extracting of Pb (II) and Mn (II) in different samples [2=
25].
In Figure 10, the re=
moval
of chromium was shown by chitosan–magnetite nanocomposite.
Fig. 10. The removal of chromium=
by
chitosan–magnetite nanocomposite strip
Magnetite particles are modified with groups such as, MPs-NH2 [=
226],
MPs–COOH [227], MPs–SH [228]. The core-shell structure of PI-b-PEG diblock
copolymer encapsulated with iron oxide nanoparticles [229]. PI-b-PEG diblock copolymer was used for
removal heavy metals from waters [230]. The
nanostructures of amphiphilic diblock copolymers due to the inherent curvat=
ure
of the polymer were shown in Figure 11 which was used for extraction lead a=
nd
other heavy metals from different matrixes.
Fig.11. The nanostructures of amphiphilic diblock copolymers for
extraction lead ions
Zero
valent iron as nanoparticles of is a Fe (0) and ferric oxide coating (nZVI)
which was used for extraction heavy metals from different matrix (Figure 3<=
/a>) [<=
/span>231]. A=
lso,
nZVI as a novel adsorbent can be removed heavy metals (Fig. 12), such as
mercury, chromium, copper, nickel, and cadmium from waters. [232-235=
]
Fig. 12. The core-shell structure of nZVI used for extraction of
metals [231]
The silica nanoparticles based on
ligand of β-ketoenol–pyridine–furan (as a selective adsorbent was used for metal removal from waters
(Pb,Cd,Zn,Cu) (Scheme 4). The engineered sorbent had high adsorption capacity=
for
capturing toxic heavy metal in environmental samples [236-239].
Scheme 4. The Silica nanoparticles based on
β-ketoenol–pyridine–furan as chelating agent for extraction heavy meta=
ls
in liquid phase
4. Conclusions
In this review pap=
er,
constructive issues from novel published papers were selected for studying =
of
separation, preconcentration, and extraction of heavy metals from water, wa=
ste
water, vegetable and human biologic samples. Recently, the SPE methods were
coupled with spectrometry techniques such as atomic absorption spectrometry
(AAS) based on various adsorbents included graphene, graphene oxide, activa=
ted
carbon, carbon nanotubes (CNTs), zeolites, MOF, magnetic nanoparticles, car=
bon
quantum dots (CQDs)a nd MSN which was used for ultra-trace determination of
heavy metals in different matrixes. In addition, the liquid-liquid micro
extraction techniques coupled with ET-AAS, F-AAS, ATF-AAS, SQT-FAAS, ICP-XR=
F,
CV-AAS, ICP,ICP-AES, ICP-MS, ICP-OES, HPLC, voltammetry, UV-VIS, and FTIR w=
ere
presented in this study by a lot of researchers. The proposed review showed=
us,
the novel techniques based on nanotechnology had been developed in SPE and =
LLE
methods since 2010 by authors. Also, SPE and solvent extraction based on
different adsorbents and instrumental techniques were extended in various
sciences such as, bio chemistry, nanotechnology, environmental analytical
chemistry and human analysis during last decade.
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