A Review On Flow Injection Analysis For Indirect Determination of Cyanide Ion in Environment by Flame Atomic Absorption Spectrometer
A Review On Flow Injection Analysis For Indirect Determination of Cyanide Ion in Environment by Flame Atomic Absorption Spectrometer
A Review On Flow Injection Analysis For Indirect Determination of Cyanide Ion in Environment by Flame Atomic Absorption Spectrometer
Peer Reviewed
Department of Chemistry, College of Education, Salahaddin University-Erbil, , Erbil, Kurdistan Region, Iraq
*Corespondance Author: hawraz.khalid@su.edu.krd
Received: 24 Jun 2022; Received in revised form: 15 Jul 2022; Accepted: 20 Jul 2022; Available online: 25 Jul 2022
©2022 The Author(s). Published by Infogain Publication. This is an open access article under the CC BY license
(https://creativecommons.org/licenses/by/4.0/).
Abstract— Among inorganic anions, cyanide is a potent toxicant in environment. Its species are
historically known as the most harmful chemical pollutants of the environment to directly affect human
health and some aquatics activity, even at minimum levels. Cyanide compounds are widely available with
various chemical compositions and are applied in many industrial fields. This mini-review focused on the
cyanide species and their measurement utilizing several analytical techniques. Detailed information on an
indirectly determined cyanide species in various environmental samples was also reviewed using a flame
atomic absorption spectrometer equipped with a flow injection system (FIA-FAAS). Obtained various
analytical performance properties of an indirectly measured free cyanide ion in various samples using
FAAS investigated from this study.
Keywords— Nonmetals, Cyanide ion, Indirect determination, FIA-FAAS.
Table 1: shows several chemical and physical properties of selected common cyanide compounds (Newhouse & Chiu, 2010;
Simeonova et al., 2004).
Formula
Cyanide Density MP BP
CASRN Synonyms (M.wt.) Form Solubility
compounds (g/mL) (°C) (°C)
g/mole
Hydrogen Hydrocyanic acid, HCN Colorless
cyanide Ether,
74-90-8 Cyclone B, gas or 0.6884 -13.4 25.7
Ethanol
prussic acid (27) liquid
2.2 Flow Injection Analysis (FIA) the volume of chemical consumption (samples and
Flow injection analysis (FIA) methods are more reagent), reduced time-wasting, and preventing lab
popular, engaging, and applicable routine analysis contamination (GHOUS, 2011; Hansen & Miró, 2007).
systems in various fields of environment applications The combination of solid-phase reagents/reactors (SPR)
(Hansen & Miró, 2007). This system provides various in FIA manifolds also provided several advantages and
exciting points, including ease of applicability, flexibility, improved this system's performances (Gomez &
reproducibility, accessibility, simplicity, an increasing Calatayud, 1998; Noroozifar, Khorasani-Motlagh, Taheri,
sampling rate, decreasing human participation, reducing & Zare-Dorabei, 2008). The utilization of the FIA-FAAS
system equipped with SPRs has been recognized and After that, Haj-Hussein, Christian, and Ruzicka (1986)
widely applied to be an effective method for automation, proposed a novel FIA system for the indirect
preparing, and analyzing various samples (Gomez & quantification of free CN- ions in aqueous systems using
Calatayud, 1998; Kapitány et al., 2020; Noroozifar et al., the AAS technique. A microcolumn, which included
2009). This coupled instrument was well applied to cupric sulfide (CuS) packed column, was proposed in the
enhance sensitivity and selectivity during nonmetal ions on-line FIA-AAS system procedure. During analysis,
or compounds analysis. The assessment of several aqueous cyanide solutions were inserted through an on-
inorganic and organic compounds has been easily line CuS packed column at a pH of 11. Simultaneously,
improved, utilizing SPR with FIA system. Many studies potassium hydroxide solution with a pH of 11 was utilized
documented the application of SPRs in the FIA-FAAS and passed into the system as a carrier stream. As a result,
system for the indirect quantification of nonmetal ions or the analyte produced the cuprocyanide complex,
compounds in various environmental samples (Gomez & presented in the eluent solution, and then measured by the
Calatayud, 1998; Hansen & Miró, 2007; Jimenez et al., FAAS detector. The consequences of sample volume,
1987; Noroozifar, Khorasani-Motlagh, & Hosseini, 2006; flow rate of the sample or used reagents and various
Zare-Dorabei et al., 2018). anionic interferences during the process were
examined.Various factors, such as carrier solution,
injection volume, flow rate, filter selection, and AAS
III. LITERATURE REVIEW
parameters, were investigated to optimize the flow system
Free cyanide and its species quantification applying and obtain reproducible results. The recorded data
FAAS was also impossible. FAAS is a powerful confirmed that the sensitivity, range of linearity, and peak
technique indirectly adopted to quantify cyanide species high could be significantly affected by the injection
in various environment samples (Dadfarnia et al., 2007; volume. In comparison with other methods, the
Gürkan & Yılmaz, 2013a; Noroozifar et al., 2009). FIA selectivity, sensitivity, applicability, and detection
equipped with the FAAS technique was a highly technique applied were introduced as the novelty of the
successful applied method to analyze free cyanide ion present method. Figures 1 and 2 illustrate detailed
indirectly. This review also focused on the indirect components of the proposed microcolumn design and
assessment and measurement of free cyanide in many filter related to the on-line FIA-FAAS system (Haj-
samples. Cyanide presented as a free ion, or total cyanide Hussein et al., 1986).
species were determined in many samples such as fish,
cocoyam, cassava, well and dam water (Kwaansa-Ansah,
Amenorfe, Armah, & Opoku, 2017), pharmaceuticals
(Gomez & Calatayud, 1998), river and sea waters
(Fullana-Barcedó, Bosch-Serrat, Marin-Saez, & Mauri-
Aucejo, 1995), and industrial wastewaters (Noroozifar,
Khorasani-Motlagh, & Hosseini, 2005). Many studies Fig.1: Illustrate the schematic diagram of FI manifold
have been documented concerning the indirect analysis associated to FIA-AAS assessment of free CN-, C, carrier;
and quantification of cyanide species using FAAS. Q, flow rate (cm3/min); S, point of injection; P, packed
Detailed analytical performance properties on the column; F, filter; M, the connection point to the
indirectly used measurement of free cyanide ion by FIA- nebulizer; AA, detector; W, waste (Haj-Hussein et al.,
FAAS in the last and this century are shown in Tables 3 1986).
and 4, respectively.
For the first time, Manahan and Kunkel (1973) proposed a
A new, sensitive, and high-speed method for extraction
simple and effective AAS procedure for indirect
(Table 3) and indirect quantification of CN-ion in various
quantification of CN- ion based upon the solubility degree
industrial samples by FAAS was also described in detail.
of copper carbonate (CuCO3) in the sample solution and
This method was proposed based on the stable producing
on the determination of the amount of copper attended to
complex of CN- ion in an alkaline medium Chattaraj and
form a cyanide-copper complex (Cu(CN)3−) in the basic
Das (1991). In the proposed method, a stable complex
medium. They applied the proposed method to quantify
species of cyanide as a [Cu(BPTC)(CN)] formed in an
low levels of cyanide at the time using the FIA system.
alkaline medium (at pH 8.2) resulting from the occurring
The spiked sample was also investigated to show the
reaction by free CN- in the sample solution with 2-
quantitative recovery of cyanide (Manahan & Kunkel,
benzoylpyridine thiosemicarbazone (BPTC). A mixture of
1973).
isobutyl methyl ketone (IBMK ) and isopentyl alcohol
with different ratios (7 + 1) was used as an appropriate Esmadi, Kharoaf, and Attiyat (1993)also described and
organic phase for extracting the stable formed complex. applied a new, simple, and potential FI-AAS method to
The analyte, which is free cyanide, converted to the stable determine cyanide and thiocyanate anions indirectly in
complex [Cu(BPTC)(CN)], extracted with high aqueous systems. At first, the silver nitrate solution used
efficiency, can be quantified indirectly by FAAS as a precipitating agent passed through the flow system
(Chattaraj & Das, 1991). and precipitated the cyanide ion (analyte) in the sample
solution in a Tygon tube coupled to the AAS detector.
Deionized water was then used to wash the formed
precipitate in the tube of the precipitating loop. Finally,
NH3 and N2S2O3 solutions, which were used as dissolving
agents, passed individually through the produced
precipitated in the Tygon tube for a short period, dissolves
the formed precipitate, and transfers it as a free cation
content to the nebulizer of the detector. As a result, the
formed cation concentration (silver ion), which is
proportionally associated with the presented quantity of
the examined analyte in the sample, could be measured
using the AAS detector. The optimum condition was
obtained due to investigate different parameters, including
the concentration of the used reagents, various
precipitating agents, washing time, and flow rate of the
chemical solutions. Compared with other previously
published methods, this method was introduced as a
preferable procedure to determine cyanide ion in
wastewater due to its simplicity, sensitivity, high
Fig.2: Shows the main components of the proposed precision, and not requiring the precipitating loop change.
microcolumn and filter related to the on-line FIA-FAAS Figure 3 illustrates the main components of the applied FI
structure (Haj-Hussein et al., 1986) system in the proposed study (Esmadi et al., 1993).
Fig.3: illustrates the principal components (schematic) of the utilized FI system to determine such as SCN - and CN- anions in
aqueous systems (Esmadi et al., 1993).
In another study,Fullana-Barcedó et al. (1995) proposed cyanide and then extraction to a new phase. The metal
two new, fast, and simple methods for the extraction complexion of Cu(CN)32- or Ag(CN)2− produced in the
(Table 3) and indirect assessment of free CN- ion in water presence of metal ions (like Cu or Ag ion) into CN-ion (at
samples via AAS techniques. They suggested this pH 10 or 11) in the sample solution, respectively. A new
procedure to produce a novel ion association compound of ion association compound [C25H46N+]2[Cu(CN)32-] or
[C25H46N+][Ag(CN)2-] formed from the reaction between electrolytic baths and pharmaceutical products. This
the metal complexion with a quaternary ammonium ion method was also preferred as a new, simple, selective, and
(benzyldimethylhexadecylammonium ion, Cetalkonium more straightforward than other previously applied FIA
chloride). Isomethylbutylketone (IBMK) solvent is then methods in the literature survey. Figure 4 illustrates the
used as an organic phase to extract the produced ion stepwise construction of the applied flow systems
association compounds. The AAS was used to measure the procedure.
cyanide ion indirectly in the final association compound stream solution; P, pump; V, valves for the sample
(Fullana-Barcedó et al., 1995). injection; BR, solid-phase reactor; and D, FAAS as a
detector (Gomez & Calatayud, 1998).
Fig.5: shows the simple components of the system combined with FAAS used to quantify free cyanide. C, carrier; P, pump;
W, waste; Inj, injector; R, it is the SPR; Hw, glass wool plug and haply nut; and D, detector(Noroozifar et al., 2005).
In addition, a practical solid-phase reactor, which consists presented as a new form of analyte in the eluent and then
of the homogenized mixture of zinc carbonate (ZnCO 3) determined by FAAS (Noroozifar et al., 2006). The
packed on silica gel beads, was also prepared and measured absorbance was increased. The used ZnCO3
suggested for indirect cyanide investigation in industrial chemical in the reactor's preparation is known as a safe,
wastewaters using FIA-FAAS. In the proposed method, cheap, stable, and readily available reagents. The results
aqueous cyanide or sample solutions were inserted onto the data confirmed that the pH of 6.0, a suitable carrier flow
on-line reactor, and the used carrier stream was re-distilled rate (2.5 mL/min), room temperature (25°C) were selected
water. Zinc cyanide complexes, which were formed as an optimal FIA system condition. Figure 6 showed the
throughout the reaction between ZnCO3 in the reactor and proposed FIA system's simple diagram with complex
free cyanide at room temperature (pH of 6.0), were components (Noroozifar et al., 2006).
Fig.6: illustrates the main components related to the proposed flow system applied to quantify free CN - ion. C, carrier; P,
pump; Inj, injector; W, waste; Hw, glass wool plug; R is an SPR; FAAS, detector(Noroozifar et al., 2006).
Furthermore,Noroozifar, Khorasani-Motlagh, and Zare- includes silver cyanide complexes formed from the free
Dorabei (2007)studied four solid-phase reactors for silver ion's reaction with the free cyanide and can then be
indirect monitoring and analyzing of free CN- ion in analyzed as a FAAS analyte. The results confirmed that the
various real industrial effluent using FIA-FAAS. The used rising in the recorded absorbance is dependable on the
solid-phase reactors were used as effectively packed changing anions in the Ag2X formula and ordered as
columns and prepared from immobilized Ag 2X (X are follows: CO3=> C2O4=> Cr2O7=> SO3=. The proposed
Cr2O72−, CO32−, C2O42−, and SO32−) mixing with silica gel method is selected as an appropriate method to determine
beads. During analysis (Figure 7), the sample solution, cyanide ion due to using Ag2X as stable, cheap reagents,
including dissolved CN- is introduced into an on-line and readily available as different forms in every laboratory
system, including Ag2X with the used deionized water or (M Noroozifar et al., 2007).
NaOH as the productive carrier stream. The eluent solution
Fig.7: illustrates the main parts of FIS combined with FAAS to quantify free CN-. CS, carrier stream; P, pump, R, solid-phase
reactor; ; ILV, injector loop valve; FAAS, detector; W, residue waste (M Noroozifar et al., 2007).
Dadfarnia et al. (2007) recommended a rapid, simple, and revealed that the suggested procedure could be readily
applicable FIS for indirect quantification of cyanide by utilized in different real samples and provide a lower
FAAS. A new microcolumn was proposed as a novel detection limit than previously documented FI-FAAS
procedure for the indirect quantification of dissolved trace methods for indirect trace quantification of CN- ion
CN ions in different aqueous systems. The column was (Dadfarnia et al., 2007).
prepared from a mixture of Salen I on sodium dodecyl A rapid FI-FAAS was additionally proposed and improved
sulfate (SDS)-coated alumina saturated with Ag(I) ion. by Noroozifar et al. (2008) for indirect quantification of
After sample injection into the microcolumn (pH 9–11), dissolved cyanide in electroplating wastewater. Various
the silver solution was formed and eluted as silver-cyanide solid phase reagents (SPRs) such as AgX (where X is N 3–,
complexes and detected by FAAS. The recorded data Br–, Cl–, and I–) were examined during analysis. In the
proposed method, five SPRs, which were mixed with SPRs for the indirect analysis of CN- ion in many
silica-gel beads and various AgX SPRs, were prepared for industrial residues (Noroozifar et al., 2008). Obtained
the final assessment. In a single-line FIA system (Figure results verified that the measurement of cyanide by the
8), the suggested procedure was depended on CN- ion proposed method appeared to be acceptable and favorable
reaction from the injected sample with immobilized AgX relative to obtained results by the previously documented
SPRs in the SPR, followed by silver formation cyanide methods. This comparison is based on several factors,
complexes in a basic medium carrier stream and later including the methods simplicity, sensitivity, speed, cost,
analysis of the eluent by FAAS. The results revealed that the limit of quantitation (LOQ), dynamic range, and
the absorbance could be increased due to changes in the relative standard deviation (RSD %). Figure 8 shows the
use of different anions as follow order: N 3-> I–> Br–> Cl–. simple FIA system's main components combined with
Based on the results, AgN3 is proposed as an effective FAAS (Noroozifar et al., 2008).
Fig.8: Shows the main parts of the FI-FAAS system for CN- analysis (C.S., carrier stream; P, pump; S, sample; SPR, reactor;
FAAS, detector; W, waste (Noroozifar et al., 2008).
In the another study, a new, cheap, simple, safe, and as an efficient extracting reagent/surfactant to the final
single-line FIA system method to indirectly quantify free complex at pH 5.5 medium (Gürkan & Yılmaz, 2013b).
cyanide in industrial wastewaters has been proposed by Gürkan and Yılmaz (2013a) also developed a novel
Noroozifar et al. (2009). The proposed method was procedure for the indirect measurement of dissolved trace
designed and applied based on the aqueous cyanide CN- employing FAAS in various real waters sample.
solution through an on-line packed column (reactor), Among them includes river water, well water, hospital
which included silver phosphate suspended on silica gel effluents, coking unit, and electroplating wastewater. In the
beads. The free silver ions are then reacted with the proposed method, the cyanide ion presence can be
presented cyanide ion in the sample solution to form the efficiently quantified utilizing FAAS after separation and
soluble complex compound in the basic medium. The preconcentration with the CPE procedure. In this method,
analyte, which is cyanide, can be indirectly measured dicyanocuprate (Cu(I) (CN)2) complex is produced due to
utilizing the FAAS instrument. The proposed method is the reduction of Cu(II) to Cu(I) with the dissolved CN- ion
appropriate for quantifying cyanide in several industrial in the sample solution. At pH 4.0, a useful ion-pairing
wastewater samples with a good detection limit, dynamic reagent (gallocyanin, GCþ) can react with the produced
range, RSD, and sample flow rate (Noroozifar et al., 2009). dicyanocuprate compound to form a new complex. The
For the first time, a cloud point extraction (CPE) method product is easily extracted by polyethyleneglycol mono-p-
was effectively applied for the isolation, preconcentration, nonylphenylether (Ponpe 7.5), extracting surfactant, and
and indirect measurement of CN- ion in several water then quantified by FAAS technique. CPE-FAAS system
samples using FAAS (Gürkan & Yılmaz, 2013b). In the was introduced as an effective indirect quantification
presence of CN- ion, the reduction of Cu(II) (coming from method for separation, preconcentration, and monitoring
the standard Cu(II) solution) to Cu(I) happens to produce trace cyanide in various aqueous systems. This technique
Cu(CN)43- complex anionic ions. Then, a new ion-associate was well-applied due to its low cost, simplicity, wide linear
complex [(NBO)3Cu(CN)4] is formed after the range, short analysis time, reasonable accuracy and
complexation reaction between the produced anionic precision, broad applicability, rejection of matrix
complex with 3-amino-7-diethylamino-8,9-benzo-2- constituents, and ease of instrumentation (Gürkan &
phenoxazine chloride (Nile blue, NB). Finally, the Yılmaz, 2013a, 2013b).
quantification analysis of cyanide is indirectly carried out Detailed analytical performance properties on the
by FAAS after using polyethyleneglycol mono-p-nonyl indirectly used measurement of free cyanide ion by FIA-
phenyl ether (PONPE 7.5). The PONPE 7.5 compound acts FAAS in the last and this century are shown in Tables 3
and 4, respectively. Analytical parameters such as methods during application based on previously documented
linear range (LR), limit of methods detection (LOD), the studies. This technique also has several valuable points
limit of quantification (LOQ), relative standard deviation associated with the economy, such as its simplicity, low-
percent (RSD%), correlation coefficient (R2), recovery, cost reagents, and high analysis speed rate. This technique
and sampling rate were shown and compared with each is preferable for the routine analytical assessments due to
other(Tables 3 and 4). Recorded results from previous its simplicity and applicability.
studies verified that FIA-FAAS could be applied to However, this method also has some disadvantages.
quantify the free cyanide in various real environmental Several parameters have to be concerned to enhance
samples (Gomez & Calatayud, 1998; Noroozifar et al., cyanide assessment while using this technique. Among
2008). In comparison with other techniques, researchers them includes controlling pH of the medium, sample or
confirmed that FIA-FAA offers promising results to reagents flow rate, carrier stream pH, and loop volume
quantify free cyanide in matrix samples (Dadfarnia et al., (Dadfarnia et al., 2007). Besides, using such reagents
2007). This technique is well known as simple, fast, widely related to toxic heavy metals can contaminate the
applicable, more sensitive, and selective, high accurate, environment (Noroozifar et al., 2005; Noroozifar et al.,
wide linear range, avoiding matrix constituent’s methods 2009; Noroozifar et al., 2008; M Noroozifar et al., 2007).
Table 3: shows the analytical performance properties of an indirectly measured free cyanide ion in various samples using FAAS
documented from the last century
Table 4: shows the analytical performance properties of an indirectly measured free cyanide ion in various samples using FAAS
documented from this century
CPE; cloud point extraction, W/ PC; with preconcentration method, W/O PC; without preconcentration method, SPR: solid-phase
reagents which are insoluble silver salts,
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