Review of Preconcentration and Solid Phase Extraction for the determination

of trace lead
Ali MOGHIMI*
Department of Chemistry, Varamin(Pishva) Branch Islamic Azad University, Varamin, Iran
* Corresponding author. e- mail: alimoghimi@iauvaramin.ac.ir
Abstract
Spectrometric techniques for the analysis of trace lead have developed rapidly due to the increasing need
for accurate measurements at extremely low levels of this element in diverse matrices. This review covers
separation and preconcentration procedures, and consider the features of the their application with several
spectrometric techniques. The use of an appropriate sample handling technique is a must in an analysis of
trace lead in water. The efforts to use a solid phase for the recovery of analytes from a water matrix prior
to their detection have a long history. The initial experimental applications of SPE resulted in widespread
use of this technique in current water analysis and also to adoption of SPE into standardized analytical
methods. Lead is recognized worldwide as a poisonous metal. Thus, the determination of this element is
often required in environmental, biological, food and geological samples. However, these analyses are
difficult because such samples contain relatively low concentrations of lead, which fall below the
detection limit of conventional analytical techniques such as flame atomic absorption spectrometry and
inductively coupled plasma optical emission spectrometry. Several preconcentration procedures to
determine lead have therefore been devised, involving separation techniques such as liquidliquid
extraction, solid phase extraction, coprecipitation and cloud point extraction. review of preconcentration
procedures for determining lead using spectroanalytical techniques. A brief overview of the history of the
use of SPE in trace lead analysis of water is given in presented paper.
Keywords : Reviews; Solid-phase extraction; Preconcentration; Water analysis; Trace lead
Contents
1. Introduction
2. The age of technical developments in trace lead analysis
3. Present status the modern age of solid-phase extraction in trace lead analysis
4. Conclusions
References
1. Introduction
Despite the selectivity and sensitivity of analytical techniques such as atomic absorption spectrometry,
there is a crucial need for the preconcentration of trace lead before their analysis due to their frequent low
concentrations in numerous samples (especially water samples). Additionally, since high levels of nontoxic components usually accompany analytes, a clean-up step is often required. Liquidliquid extraction
is a classical method for preconcentrating metal ions andyor matrix removal. Solid phase extraction (SPE)
is another approach that offers a number of important benefits. It reduces solvent usage and exposure,
disposal costs and extraction time for sample preparation. Consequently, in recent years SPE has been
successfully used for the separation and sensitive determination of metal ions, mainly in water samples.
After outlining the theory of this technique, guidelines are given for the development of SPE-based
methods for preconcentration of many trace lead. Finally, examples of applications are presented.
From the analytical tools above listed, FAAS presents low costs, operational facility and high sample
throughput. The determination of cadmium by flame atomic spectrometry is free of interference and this
can be easily atomized in air-acetylene flame. In the resonance line 228 nm, the characteristic
concentration is 0.02 mg L1. The analytical line at 326.1 nm is suitable for determining higher Cd
1

concentrations and the characteristic concentration is about 6mg L1, so that excessive dilution can be
avoided [15]. Cadmium can be determined by CV AAS where atomic Cd vapor is measured by AAS in
an unheated quartz cell. LOD of 80 ng L1 was obtained which can be further improved by working at
low temperature. The sensitivity can be increased collecting the atomic Cd vapor in a graphite tube pretreated with palladium at 150 C and then reatomizing at 1600 C [14]. Cold vapor generation coupled to
atomic absorption spectrometry with flow injection (FI-CV AAS) was evaluated as a rapid and simple
method for the determination of cadmium [16]. The determination of cadmium by ETAAS was, for a long
period, difficulty because the cadmium is an element with high volatility [17].
The principle of SPE is similar to that of liquid liquid extraction (LLE), involving a partitioning
of solutes between two phases. However, instead of two immiscible liquid phases, as in LLE, SPE
involves partitioning between a liquid (sample matrix) and a solid (sorbent) phase. This sample treatment
technique enables the concentration and purification of analytes from solution by sorption on a solid
sorbent. The basic approach involves passing the liquid sample through a column, a cartridge, a tube or a
disk containing an adsorbent that retains the analytes. After all of the sample has been passed through the
sorbent, retained analytes are subsequently recovered upon elution with an appropriate solvent. The first
experimental applications of SPE started fifty years ago [1,2,3]. However, numerous studies have also
shown the great potential of this technique for speciation studies.[18,161-177]
1.1. Basic principles
An SPE method always consists of three to four successive steps, as illustrated in Fig. 1. First, the solid
sorbent should be conditioned using an appropriate solvent, followed by the same solvent as the sample
solvent. This step is crucial, as it enables the wetting of the packing material and the solvation of the
functional groups. In addition, it removes possible impurities initially contained in the sorbent or the
packaging. Also, this step removes the air present in the column and fills the void volume with solvent.
The nature of the conditioning solvent depends on the nature of the solid sorbent. Typically, for reversed
phase sorbent (such as octadecyl-bonded silica), methanol is frequently used, followed with water or
aqueous buffer whose pH and ionic strength are similar to that of the sample. Care must be taken not to
allow the solid sorbent to dry between the conditioning and the sample treatment steps, otherwise the
analytes will not be efficiently retained and poor recoveries will be obtained. If the sorbent dries for more
than several minutes, it must be reconditioned.
The second step is the percolation of the sample through the solid sorbent. Depending on the system used,
volumes can range from 1 ml to 1 l. The sample may be applied to the column by gravity, pumping,
aspirated by vacuum or by an automated system. The sample flow-rate through the sorbent should be low
enough to enable efficient retention of the analytes, and high enough to avoid excessive duration. During
this step, the analytes are concentrated on the sorbent. Even though matrix components may also be
retained by the solid sorbent, some of them pass through, thus enabling some purification (matrix
separation) of the sample.
The third step (which is optional) may be the washing of the solid sorbent with an appropriate solvent,
having a low elution strength, to eliminate matrix components that have been retained by the solid
sorbent, without displacing the analytes.

Fig. 1. SPE operation steps.

2

A drying step may also be advisable, especially for aqueous matrices, to remove traces of water from the
solid sorbent. This will eliminate the presence of water in the final extract, which, in some cases, may
hinder the subsequent concentration of the extract andyor the analysis. The final step consists in the
elution of the analytes of interest by an appropriate solvent, without removing retained matrix
components. The solvent volume should be adjusted so that quantitative recovery of the analytes is
achieved with subsequent low dilution. In addition, the flow-rate should be correctly adjusted to ensure
efficient elution. It is often recommended that the solvent volume be fractionated into two aliquots, and
before the elution to let the solvent soak the solid sorbent.
1.2. Retention of trace lead on the sorbent
Adsorption of trace lead on the solid sorbent is required for preconcentration (see Fig. 2). The mechanism
of retention depends on the nature of the sorbent, and may include simple adsorption, chelation or ionexchange. Also, for trace lead, ion-pair solid phase extraction may be used.
1.2.1. Adsorption.
Trace lead are usually adsorbed on solid phases through van der Waals forces or hydrophobic interaction.
Hydrophobic interaction occurs when the solid sorbent is highly non-polar (reversed phase). The most
common sorbent of this type is octadecyl-bonded silica (C18 -silica). More recently, reversed polymeric
phases have appeared, especially the styrene-divinylbenzene copolymer that provides additional pp
interaction when p-electrons are present in the analyte w4x. Elution is usually performed with organic
solvents, such as methanol or acetonitrile. Such interactions are usually preferred with online systems, as
they are not too strong and thus they can be rapidly disrupted. However, because most trace element
species are ionic, they will not be retained by such sorbents.
1.2.2. Chelation.
Several functional group atoms are capable of chelating trace lead. The atoms most frequently used are
nitrogen (e.g. N present in amines, azo groups, amides, nitriles), oxygen (e.g. O present in carboxylic,
hydroxyl, phenolic, ether, carbonyl, phosphoryl groups) and sulfur (e.g. S present in thiols,
thiocarbamates, thioethers). The nature of the functional group will give an idea of the selectivity of the
ligand towards trace lead. In practice, inorganic cations may be divided into 3 groups:
group I-hard cations: these preferentially react via electrostatic interactions (due to a gain in
entropy caused by changes in orientation of hydration water molecules); this group includes alkaline and
alkaline-earth metals (Ca2+ , Mg2+ , Na+ ) that form rather weak outer-sphere complexes with only hard
oxygen ligands.
group II-borderline cations: these have an intermediate character; this group contains Fe , Co2+ Ni2+
Cu2+ Zn2+ Pb2+ Mn2+ . They possess affinity for both hard and soft ligands. group III-soft cations:
these tend to form covalent bonds. Hence, Cd2+ and Hg2+ possess strong affinity for intermediate (N)
and soft (S) ligands.
For soft metals, the following order of donor atom affinity is observed: 0-N-S. A reversed order is
observed for hard cations. For a bidentate ligand, affinity for a soft metal increases with the overall
softness of the donor atoms: (0, 0)-(0, N)-(N, N)-(N, S). The order is reversed for hard metals. In general,
the competition for a given ligand essentially involves Group I and Group II metals for O sites, and
metals of Group II and Group III for N and S sites. The competition between metals of Group I and
Group III is weak.
Chelating agents may be directly added to the sample for chelating trace lead, the chelates
being further retained on an appropriate sorbent. An alternative is to introduce the functional chelating
group into the sorbent. For that purpose, three different means are available: (1) the synthesis of new
sorbents containing such groups (new sorbents); (2) the chemical bonding of such groups on existing
sorbents (functionalized sorbents); and (3) the physical binding of the groups on the sorbent by
impregnating the solid matrix with a solution containing the chelating ligand (impregnated, coated or
loaded sorbents). The latter remains the most simple to be used in practice. Its main drawback is the
possible flush of the chelating agent out of the solid sorbent

during sample percolation or elution that reduces the lifetime of the impregnated sorbent. Different
ligands immobilized on a variety of solid matrices have been successfully used for the preconcentration,
separation and determination of trace metal ions. Chelating agents with an hydrophobic group are retained
on hydrophobic sorbents (such as C18 -silica). Similarly, ion-exchange resins are treated with chelating
agents containing an ionexchange group, such as a sulfonic acid derivative of dithizone (i.e.
diphenylthiocarbazone) (DzS), 5-sulfo-8-quinolinol, 5-sulfosalicylic acid, thiosalicylic acid, chromotropic
acid, or carboxyphenylporphyrin (TCPP) [58]. Binding of metal ions to the chelate functionality is
dependent on several factors: (1) nature, charge and size of the metal ion; (2) nature of the donor atoms
present in the ligand; (3) buffering conditions which favor certain metal extraction and binding to active
donor or groups; and (4) nature of the solid support (e.g. degree of cross-linkage for a polymer). In some
cases, the behavior of immobilized chelating sorbents towards metal preconcentration may be predicted
using the known values of the formation constants of the metals with the investigated chelating agent [9].
However, the presence of the solid sorbent may also have an effect and lead to the formation of a complex
with a different stoichiometry than the one observed in a homogeneous reaction [10,11]. In fact, several
characteristics of the sorbent should be taken into account, namely the number of active groups available
in the resin phase [7,10], the length of the spacer arm between the resin and the bound ligand [12], and the
pore dimensions of the resin [13].

Fig. 2. Interactions occurring at the surface of the solid sorbent. F, functional group; TE, trace element;
MS, matrix solvent; MI, matrix ions; ES, elution solvent.

2. Lead determination
2.1. Atomic absorption spectrometry (AAS)
The determination of lead by flame atomic absorption spectrometry (FAAS) is practically free of
interference and requires an airacetylene flame [13]. The interference caused by aluminum and
iron can be overcome by the addition of ascorbic acid, citric acid and EDTA [13]. The threshold
of sensitivity of this technique is very low (LOD 0.01 mg L1) and is often unsuitable for trace
analysis [13]. In this sense, many preconcentration procedures must be performed to determine
trace amounts of lead, as indicated in the tables shown here. The most important analytical lines
of lead are 217.00 and 283.31 nm. The 217.00 nm line is more sensitive, notwithstanding the
greater amount of background absorption effects [13].
Electrothermal atomic absorption spectrometry (ETAAS) is a good alternative for determining
trace amounts of lead in several types of samples in view of its good sensitivity [13]. However,
in some cases, previous preconcentration and separation steps are carried out before analytical
measurements by ETAAS.
The use of a modifier stabilizes lead, allowing for its determination without causing matrix
effects. The PdMg modifier is the one most commonly used, since it produces the best results.
This modifier allows for the application of pyrolysis temperatures ranging from 1200 to 1400 C,
which enables the separation of most interfering elements [1317]. The stabilizing effect of this
modifier also raises the atomization temperature to 2000 C, which allows a characteristic mass
of about 16 pg [13]. Ammonium phosphate is another modifier frequently used for determining
lead by ETAAS, allowing for an atomization temperature of 1600 C and enabling a low
characteristic mass of 12 pg [13,18].
2.2. Inductively coupled plasma optical emission spectrometry (ICP OES)
Inductively coupled plasma optical emission spectrometry is an analytical technique often
employed to determine lead in various types of samples [19]. The main emission lines are: Pb II
220.353 nm, Pb I 216.999 nm and Pb I 283.306 nm, with 220.353 nm being the most sensitive.
However, the low level of lead in many samples lies below the detection limit of this technique.
Moreover, several types of spectral interference have been reported in the determination of lead
by ICP OES. Virtually all photomultiplier-based ICP spectrometers use the Pb 220.353 nm
analytical line, despite its severe background continuum and inter-element interference from Al
220.4 nm and background shift due to iron (Fe). Direct spectral overlap interference due to iron
has also been found in the 216.9 and 283.9 nm analytical lines [20,21]. Thus, preconcentration
and separation procedures have been devised to allow trace amounts of lead to be determined in
complex matrices using ICP OES. Several tables shown in this paper summarize the use of
separation techniques such as liquidliquid extraction, solid phase extraction, cloud point
extraction and others, as pre-steps in determining lead using ICP OES.
3. Lead separation and preconcentration
Separation techniques such as coprecipitation [23,50], liquidliquid extraction [5760], solid
phase extraction [69134] and more recently, cloud point extraction [139146,150] and on-line
coprecipitation using a knotted reactor [150160] have been successfully employed to determine
trace levels of lead. Each technique has its pros and cons and should be chosen according to the
analytical problem.

3.1. Coprecipitation
5

Coprecipitation is one of the most efficient separation/ enrichment techniques for trace heavy
metal ions. The main requirement for this technique is that the collector should separate easily
from the matrix solution. This can be done by filtering, centrifuging and washing of the
precipitate. In addition, it is desirable that the collector should be a pure and readily available
substance. The advantages of this technique are its simplicity and the fact that various analyte
ions can be preconcentrated and separated simultaneously from the matrix. Inorganic or organic
coprecipitants have been used as efficient collectors of trace elements. However, this process is
slow and samples sometimes have to be kept over-night for complete coprecipitation [22]. This
technique has been widely applied in preconcentration procedures for determining lead inwater
samples. Inorganic coprecipitants such as manganese dioxide and aluminum, gallium,
cerium(IV), erbium, iron(III), magnesium, samarium and zirconium hydroxides have been
widely and successfully used for preconcentrating trace lead ions from different mediums
[23,50]. A fast procedure for separation and preconcentration using ultrasound-assisted
coprecipitation with manganese dioxide has recently been proposed for determining lead in
environmental samples by ICP OES [18]. Coprecipitation parameters, including concentration of
oxidizing agentKMnO4, concentration of MnSO4 and exposure time to ultrasound irradiation,
are discussed. The time required for coprecipitation is about 60 s.
Another paper proposed an aluminum hydroxide coprecipitation method for the determination of
trace amounts of Cu, Cd and Pb by FAAS in seawater and mineral water after a 125-fold
preconcentration [19]. Table 1 lists several methods for determining lead in many samples, using
coprecipitation as the separation and preconcentration technique
3.2. Liquidliquid extraction
Solvent extraction has been one of the most extensively studied and widely applied methods in
preconcentration and separation procedures for the determination of trace elements due to its
simplicity, convenience, wide scope, etc. In this technique, the metal is distributed between two
immiscible liquid phases (usually an aqueous and an organic phase). Metal ion stripping from
aqueous solution to organic phase takes place after a complexation reaction. For the analytical
measurement, the extracted metal ion can be directly measured in organic extract or a
backextraction step is carried out in an aqueous medium, usually acid [5153]. Separation and
preconcentration procedures using solvent extraction generally result in a high enrichment factor
due to the difference between the volumes of aqueous and organic phases. Although this
procedure is operated in batch mode, it is time-consuming and produces large amounts of
potentially toxic organic solvents as waste. The implementation of methods in continuous mode
overcomes these drawbacks. Such unit operations are, instead, carried out in flow injection (FI)
and/or sequential injection (SI) systems, which, besides reducing sample and reagent
consumption, allow all manipulations to be done automatically in an enclosed environment, thus
minimizing the risk of sample contamination. Analytical procedures for lead separation and
preconcentration by solvent extraction and determination by atomic spectrometric techniques
have been widely applied since these techniques were invented [54].

Table 1
Preconcentration procedures using coprecipitation for the determination of lead

Table 2
Procedures for lead preconcentration based on solvent extraction

Procedures in flow injection systems for separation and preconcentration with the application of
solvent extraction to determine metals, including lead, are extensively discussed in the literature
[55,56]. Table 2 lists several analytical systems proposed for lead separation and
preconcentration by solvent extraction and lead determination using atomic spectrometric
techniques.

3.3. Solid phase extraction

Solid phase extraction is based on the partition between a liquid (sample matrix) and a solid
phase (sorbent). Several sorbents coupled to detection systems have been used for lead
preconcentration and determination. The basic approach is the contact of a liquid sample through
a column, a flask, a cartridge, a tube or a disk containing an adsorbent that retains lead ions.
After this first step, the retained lead is recovered upon elution with an appropriate solvent [68].
Sorbents used in preconcentration systems for lead determination can be unloaded, loaded or
chemically modified with the help of complexing reagents. Unloaded supports are potential
collectors of analytes in the form of a single ion or associated with other species such as
complexes. The sorbents in this class include activated carbon [69], natural adsorbents [70],
Amberlite XAD resins [7175], polyethylene [76] and others [77]. Lead can also be complexed
with ligands loaded in several supports, such as polyurethane foam [7880], activated carbon
[81] and polymeric materials [8284], which make for efficient preconcentration procedures.
Many reagents have been used to load these supports and to retain lead ions by complexation.
These include: 2-(2_-thiazolylazo)-pcresol (TAC) [85], 2-propylpiperidine-1-carbodithioate [86],
2-(2-benzothiazolylazo)-2-p-cresol (BTAC) [80,87], pyrogallol red [81], 1-(2-pyridylazo)-2naphthol (PAN) [88], dithizone [89,90] and 2-(5-bromo-2-pyridylazo)-5-diethyl-aminophenol (5Br-PADAP) [91]. Supports can also be functionalized with chelating reagents, which render
them powerful absorbents for lead preconcentration. Supports such as Amberlite XAD series
[92,93], silica gel [9496] and cellulose [97,84] have been modified with reagents by several
routes. Several methods have been proposed for preconcentrating lead using the solid phase
batch extraction procedure (Table 3).

3.4. Automation and possible on-line coupling toanalysis techniques

SPE can be easily automated, and several commercially available systems have been recently
reviewed [123]. Home-made systems have also been reported [124]. In addition, all the sample
volume is further analyzed, which enables smaller sample volume to be used. However, in the
case of complex samples, off-line SPE should be preferred due to its greater flexibility, and the
opportunity to analyze the same extract using various techniques.
3.4.1. On-line coupling to liquid chromatography.
On-line systems mainly use a micro-column. The sorbent is chosen not only for its efficiency in
trapping analytes, but also for its compatibility with the stationary phase packed into the
chromatographic column. Indeed, it is highly recommended to use the same packing in the
precolumn and the chromatographic column to prevent losses in efficacy upon analysis. For the
case of two different sorbents being used, the retention of the analytes in the precolumn should
be lower than in the analytical column to ensure band refocusing at the head of the
chromatographic column. On-line systems with several detectors have been reported, such as
ultraviolet (UV) detector or inductively coupled plasma mass spectrometer (ICP MS), with
detection limits in the 0.0550 mgyl range. Detection limits as low as 0.5 ngyl could even be
achieved by detection at the maximum absorption wavelength using a photodiode array UV
detector [125].

3.4.2. On-line coupling to atomic absorption

8

spectrometry. Olsen et al. [126] and Fang et al .[127,128] were the first to describe an on-line
flowinjection (FI) sorbent extraction preconcentration system for flame AAS (F-AAS) using
microcolumns packed with a cation-exchanger. Later, they also proposed a system for on-line
flowinjection sorbent extraction preconcentration with electrothermal vaporization AAS (ETAAS) using lead as a model trace element[129]. Since then, numerous papers reported FI with
on-line preconcentration followed by AAS, as exemplified by determination of Pb [129].
Selected applications are reported in Table 4. The sorbent should provide for rapid sorption and
desorption of the analytes to be used in FI systems [130]. In addition, it should be provided for a
high selectivity. In practice, C18-silica is very frequently used as organic solvents (such as
methanol) can be used as eluting solvents leading to a high sensitivity in flame AAS.
Complexing reagents are, therefore, added for efficient retention of trace metals. Their choice is
based on their fast reaction with metals, such as diethyldithiocarbamate (DDTC) and ammonium
pyrrolidine dithiocarbamate (APDC) [131,132]. In addition, both reagents are water soluble and
do not adsorb on C18-silica so that it does not overload with the reagent itself. However, these
reagents lack selectivity, so that other reagents have been used for particular applications, like 110-phenanthroline [135s], 0,0-diethyl-dithiophosphate (DDTP) [134]. The micro column can be
inserted into the tip of the PTFE capillary in the autosampler arm of a graphite furnace atomic
absorption spectrometer [131]. Even though C18-silica has been the most frequently used
sorbent for FI preconcentration, other sorbents were found satisfactory for some applications as
shown in Table 4, such as functionalized activated carbon [134], polyurethane foam (PUF) [134],
or PTFE turnings [133]. A particular knotted reactor (KR) has been recently developed, which
consists of a long tube properly knotted usually made of PTFE.
3.4.3. On-line coupling to ICPAES or ICP MS.
The first report of FI on-line preconcentration coupled to ICP-atomic emission spectrometry
(AES) appeared nearly twenty years ago [130]. Since then, several studies have used this
coupling with different sorbents such as ZrO2 or functionalized silica gel for example [136].
3.4.4. On-line coupling to spectrophotometry.
Spectrophotometry offers the advantage of requiring inexpensive and very common
instrumentation. In addition, by choosing a non-selective chromogenic reagent, multi-metal
determinations may be possible[123]. Its coupling to FI analysis is well suited for monitoring
purposes and a few studies present such systems as indicated in Table 4 [123]. Solid-phase
spectrophotometry (SPS) has also been reported with FI systems due to its simplicity and low
detection limits. The solid sorbent is packed in either commercially available or customized flow
cells. On-line FI sorbent extraction procedures have several advantages over the corresponding
off-line methods: higher sample throughput (increased by 1 to 2 orders of magnitude), lower
consumption of sample and reagent (also reduced by 1 to 2 orders of magnitude), better precision
(with relative standard deviations approx. 12%), lower risk of loss or contamination and easy
automation.
3.5. Cloud point extraction (CPE)
The cloud point phenomenon occurs when a nonionic or amphoteric surfactant above its critical
micellar concentration (CMC) causes the separation of the original solution into two phases
when heated at a characteristic temperature called cloud point temperature. Above the cloud
point, micelles formed from surfactant molecules act as an organic solvent in liquidliquid
9

extraction and the analytes are partitioned between the micellar and aqueous phases [135137].
Thus, metallic elements can be extracted to a surfactant-rich phase, trapped in the hydrophobic
micellar core, in the form of hydrophobic complexes that are formed between the metal ion and
an appropriate chelating agent under adequate conditions. An evaluation of the partition
coefficients of ligands and complexes involved is, therefore,
Table 3
Off-line procedures for lead preconcentration using solid phase extraction

Table 4
10

Applications of SPE to FI on-line preconcentration systems

Matrix

Sorbent

Eluent

Analysis method

Recovery%

LOD(ng/l)

Ref.

99.2101%

Preconcentration
factor
60189

Certified
biological,
vegetable
samples
Standard
solutions
Standard
solutions
Tap, river and
coastalwaters,
marine
sediment,
fish and
mussel
tissues
Standard
solutions
River, ground
waters

C18-silica

IBMK

F-AAS

3000

[132]

C18-silica

EtOH

F-AAS

--

41000

3003000

[134]

C18-silica

MeOH

F-AAS

--

1460

4000-10000

[130]

PTFE
turnings

IBMK

F-AAS

95102

330

800

[133]

PUF

EtOH

F-AAS

--

41000

3003000

[134]

Lewatit
TP80784
PAPhA

HCl

Spectrophotometry

80120

50

2000-5500

[123]

Table 5
CPE applications for lead preconcentration and determination

TAN: 1-(2-Thiazolylazo)-2-naphthol; Br-PADAP: 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol; DDTP: O,O-diethyldithiophosphate

Table 6
Separation and preconcentration of lead using knotted reactors.

ng L1.

11

Surfactant solutions provide a medium that modifies the reaction ratio, equilibrium position and
spectral and analytical parameters. However, the micellar phase obtained after a CPE has
physical and chemical characteristics that must be taken into account in the development of an
analytical procedure. Borges et al. [140], for example, determined lead by preconcentration in a
micellar phase of Triton X-114 and determination by ETAAS using Ir and Ru as permanent
modifiers. This enabled them to reach a higher pyrolysis temperature and thus, eliminate the
surfactant matrix before the atomization step without risk of analyte loss, as well as to avoid high
background absorption. Table 5 shows some recent CPE applications for lead determination and
some analytical characteristics.
4. Conclusions
Considering the poisonous nature of lead and the low concentration of this element in samples,
preconcentration procedures have been devised involving separation techniques such as liquid
liquid extraction, solid phase extraction, coprecipitation and cloud point extraction. Nevertheless,
each technique has its pros and cons and should therefore be chosen according to the analytical
problem. Most of the proposed methods were established using solid phase extraction. In recent
years, on-line systems have been preferred.
Acknowledgements
The author gratefully acknowledge department of chemistry, Varamin(Pishva) branch Islamic
Azad University, Varamin.
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