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Original Article
10 (
2_suppl
); S2090-S2097
doi:
10.1016/j.arabjc.2013.07.040

Chemically functionalized γ-alumina with Alizarin red-s for separation and determination of trace amounts of Pb(II) and Ag(I) ions by solid phase extraction–Flame Atomic Absorption Spectrometry in environmental and biological samples

, , , ,
 Department of Chemistry, Payame Noor University (PNU), Shiraz 71365-944, Iran

⁎Corresponding author. Tel.: +98 9173153520; fax: +98 7116222249. Tavallali@yahoo.com (Hossein Tavallali) Tavallali@pnu.ac.ir (Hossein Tavallali)

Received: , Accepted: ,
© The Author(s) 2013
Disclaimer:
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.

Peer review under responsibility of King Saud University.

Abstract

A novel column solid phase extraction was developed for the determination of traces of lead and silver in various samples. An alumina–sodium dodecyl sulfate (SDS) coated on with Alizarin red-s was used for preconcentration of lead and silver ions prior to determination by flame atomic absorption spectrometry. Lead and silver were adsorbed quantitatively on a modified column due to its complexation with Alizarin red-s and then eluted using 5.0 mL 4.0 mol L−1 phosphoric acid. The influences of the analytical parameters such as pH, solid phase amount, ligand amount, types and concentration of eluting agent were investigated. The loading capacity of adsorbent for Pb and Ag were found to be 2.3 and 2.1 mg g−1. The detection limits were 18.0 and 55.0 μg L−1 for lead and silver respectively, applying a preconcentration factor of 100.0. The relative standard deviation under optimum conditions is lower than 2.0%. The presented procedure was successfully applied for the determination of analytes content in real samples. The results were obtained and are in good agreement with the reported method.

Keywords

Solid phase extraction
Sodium dodecyl sulfate (SDS)
Flame atomic absorption spectrometry
Alizarin red-s
1

1 Introduction

The roles of transition elements at trace level in the human body are an important search subject of an analytical chemist (Pyrzynska, 2007; Duran et al., 2007; Szentmihalyi et al., 2007). The line between the quantity being indispensable and harmful is very limited. Heavy metal ions should be accurately evaluated in order to prevent the occurrence of harmful effects. The cycle of trace metal ions from environment to human is also an important part of environmental studies (Afridi et al., 2007; Jamali et al., 2007; Ramesh et al., 2001; Sarica and T¨urker, 2007). Flame atomic absorption spectrometry (FAAS) is one among common techniques for heavy metals determination because it offers many advantages (Berman, 1980) but direct determination of trace heavy metals such as lead and silver in real samples by it is not always possible, due to matrix interferences and very low concentrations of metal ions, therefore a preconcentration/separation step is required (Klassen et al., 1986; Marczenko, 1986; Welz, 1985), and is of special importance (Mortatti et al., 1982) in order to bring the concentration of the analyte within the dynamic measuring range of the detection limit. The separation enrichment techniques have been used to improve the sensitivity and selectivity of the trace analysis of the metal ions. Few methods like solvent extraction (Lajunen and Kubin, 1998), electro-deposition (Cansky et al., 2007), coprecipitation (Saracoglu et al., 2001), cloud point extraction (Ebihara et al., 2007), membrane filtration (Karatepe et al., 2002) and solid phase extraction (Dogan and Akcin, 2007; Soylak et al., 1999; Karabelli et al., 2011; Mahmoud et al., 2008; Morsi et al., 2010) have been reviewed for the enrichment of heavy metal ions. Solid phase extraction (SPE) based on the adsorption is also one of the important preconcentration methodologies. It has some advantages including short analysis time, high preconcentration factor, and low consumption of the organic solvent. Therefore it can provide more flexible working conditions and simple operation (Arrebola Ramirez et al., 1994). SPE is mainly based on the utilization of inorganic and organic solid sorbents such as XAD resins (Ferreira et al., 2000), SDS-coated alumina (Ghaedi, 2006a; Ghaedi et al., 2006b), active carbon (Pena et al., 1995) and others (Szezepaniak and Jskowiak, 1982).

These sorbents are well known and mainly based on the possible surface reactivity and adsorptive characters incorporated into these solid phases (Sakai et al., 1986).

The purpose of this work was to investigate the selective absorption of lead and silver ions on SDS-coated alumina modified with Alizarin red-s and later analysis by flame atomic absorption spectrometry. The effective parameters such as pH of sample, amount of solid phase, type and concentration of eluting agent were optimized. The proposed method is also applied to the determination of the analytes in environmental and biological samples.

2

2 Experimental

2.1

2.1 Instrumentation

A Sens AA GBC double beam atomic absorption spectrometry (AAS) with air-acetylene flame and hallow cathode lamps was used for the analysis of lead and silver. A deuterium lamp was used for background correction. All instrumental settings were those recommended in the manufacturer’s manual book and the instrumental conditions are shown in Table 1. A suction pump (Watson–Marlow, Falmouth, UK; model 101/U/R) was used to adjust the flow rate. The open microwave system was purchased from Daewoo Company (Korea) model KOC-1BOK. The pH measurements were carried out using a Jenway pH meter (model 3510) with a combined pH glass electrode calibrated against two standard buffer solutions at pH 4.0 and 7.0.

Table 1 Instrumental conditions for the measurements of the analyst by FAAS.
Analyte Wavelength (nm) Slit width (nm) Lamp current (mA)
Pb 217.0 1.0 5.0
Ag 328.1 0.5 4.0

2.2

2.2 Reagents and standard solution

All chemicals used in this work, were of analytical-reagent grade (Merck) and were used without further purification. Doubly distilled deionized water was used for all dilutions. All plastic and glassware were cleaned by soaking in dilute HNO3 (1 + 10) and were rinsed with distilled water prior to use. The element standard solutions of 1000.0 mg L−1 of the given element were supplied by Merck. Stock solutions of diverse elements were prepared from high purity compounds. The γ-Al2O3 mesh 10.0–50.0 was purchased from Merck Company and used as received.

2.3

2.3 Chemically functionalized γ-alumina with Alizarin red-s

A 10.0 mL volume of SDS-Alizarin red-s solution was added to 40.0 mL of water solution containing 0.7 g alumina particles. The pH was adjusted to 6.0 with the addition of 2.0 mol L−1 hydrochloric acid to form Alizarin-impregnated ad-micelles on alumina particles while shaking the suspension with a stirrer. The mixture was then filtered, washed, air-dried, and stored in a closed brown bottle for subsequent use.

2.4

2.4 Column preparation

A glass column with an inner diameter of 1.0 cm and a length of 10.0 cm, equipped with porous frits, was filled up to a height of about 2.0 cm with a suspension of SDS coated on alumina modified with Alizarin red-s in water. A little glass wool was placed at the both ends to retain the sorbent in the tube. SDS coated on alumina modified with Alizarin red-s was preconditioned by the blank solution prior to each use. After each experiment, the column was rinsed with water and stored for the next experiment.

2.5

2.5 Test procedure

The pH of 500.0 mL of solution containing 100.0 μg L−1 of the each analyte was adjusted to pH 6.0 with 0.1 mol L−1 NaOH and was passed through the Alizarin red-s coated alumina column at a flow rate of 2.0 mL min−1 with the aid of a suction pump. The retained ions adsorbed on the column were eluted with 5.0 mL of H3PO4 solution (4.0 mol L−1) at an elution rate of 2.0 mL min−1. The lead and silver ions concentration in the eluent solution, were determined by FAAS.

2.6

2.6 Analysis of real samples

2.6.1

2.6.1 Wastewater sample

Analysis of wastewater sample (from Shiraz Petrochemical Company-Iran) for the determination of analyte contents was performed as following: 400.0 ml of sample was poured in a beaker and 8 ml concentrated HNO3 and 3.0 ml of H2O2 of (30%) for the elimination and decomposition of organic compound were added. The samples, while stirring were heated to one-tenth volume (Ghaedi et al., 2007). After adjustment of the final solution to pH 6.0, the procedure given in Section 2.5 was performed.

2.6.2

2.6.2 Soil and blood samples

20.0 g (soil sample) or 20.0 mL (blood sample) was weighed accurately and in a 200.0 ml beaker was digested with the addition of 10.0 ml concentrated HNO3 and 2.0 ml HClO4 70% was added and heated for 1.0 h. The content of the beaker was filtered through a No. 40 filter paper into a 250.0 ml calibrated flask and its pH was adjusted to the desired value and diluted to the mark with deionized water (Ghaedi et al., 2007). Then the procedure given in Section 2.5 was performed.

2.6.3

2.6.3 Amalgam sample

The commercial form of the amalgam takes the form of little balls, each weighing 1.0 g. One of these exactly weighing balls was dissolved in 1:1 HNO3 and the mixture was carefully boiled until complete dissolution of the amalgam was achieved. The pH was adjusted to 6.0 and diluted by appropriate dilution of the mother solution to 100.0 mL (Haji Shabani et al., 2009).

2.6.4

2.6.4 Hair sample

The human hair sample was rinsed with acetone, chloroform and doubly distilled water and then was dried at 60.0 °C. An exact weight of sample (0.5 g) was treated with 12.0 mL of concentrated HNO3 and 2.0 mL concentrated HClO4 and was heated on a hot plate at 150.0 °C for 30.0 min. Finally, about 5.0 mL of 30% H2O2 solution was gradually added until the solution turned colorless and was heated nearly to dryness at 200.0 °C to yield a whitish residue. Approximately 5.0 mL of 0.1 mol L−1 HNO3 was added to the baker and the contents were heated at 100.0 °C for 15.0 min. The pH of solution was adjusted to 6.0 and was diluted to 100.0 mL in a conical flask (Ghaedi et al., 2009).

2.6.5

2.6.5 Mushroom sample

One gram of mushroom sample was digested with 6.0 mL of HNO3 (65%) and 2.0 mL of H2O2 (30%) in microwave digestion system and diluted to 10.0 mL with deionized water. A blank digest was carried out in the same way. Digestion conditions for microwave system for all samples were applied as 2.0 min for 250 W, 2.0 min for 0 W, 6.0 min for 250 W, 5.0 min for 400 W, 8.0 min for 550 W, and ventilation 8 min, respectively. The preconcentration procedure given in Section 2.5 was applied to the samples (Soylak et al., 1995).

3

3 Results and discussion

To obtain the most suitable data from this method, different parameters were optimized. The pH of sample solution, amount of ligand and solid phase, type of eluting agent and its concentration, interfering effect of coexisting ions and maximum capacity of the sorbent for lead and silver ion recovery, have been studied. The optimization procedure was carried out by varying a parameter while the others were kept constant.

3.1

3.1 Influences of pH

The pH of the working media is a main analytical factor for the quantitative recoveries of metal ions by solid phase extraction (Hiraide et al., 1995; Karve and Rajgor, 2009; Kalfa, 2009). The effect of pH on the preconcentration of metal ions on SDS coated on alumina modified with Alizarin red-s was studied by the determination of individual elements. The pH value of the sample solutions was adjusted to a pH range of 3.0–8.0 with a universal buffer. In all cases, metal retention by the reagent increased with increasing pH and reached a maximum at pH 6.0 after which the retention decreased. The decrease in signal at pH > 6.0 is probably due to the precipitation of ions as their related hydroxide precipitates or complexes and at pH < 6.0 may be due to the competition of hydronium ion toward complexation with Alizarin red-s which leads to the decrease in the recovery, so pH 6.0 was chosen for the further studies and graphically represented in Fig. 1.

Influences of pH on recovery of metal ions (N = 3).
Figure 1
Influences of pH on recovery of metal ions (N = 3).

3.2

3.2 Effect of the amount of adsorbent

Sorption of SDS on α-alumina over a wide range of pH (3.0–8.0) is very slight, probably because of its chemically inert surface (Merino et al., 2003). Thus, the use of γ-alumina is essential for the preparation of chelating sorbent. Fig. 2 illustrates the effect of the amounts of alumina filled to the column on recoveries of lead and silver. The retention of the metal ions was examined in relation to the amount of adsorbent, which was varied from 50.0 to 150.0 mg. It was found that the recoveries of lead and silver gradually increased up to 75.0 mg of the adsorbent. Therefore, 75.0 mg of the adsorbent was used for lead and silver.

Effect of the amount of adsorbent on recovery of metal ions (N = 3).
Figure 2
Effect of the amount of adsorbent on recovery of metal ions (N = 3).

3.3

3.3 Amount of SDS

The effect of amounts of SDS on the recoveries of the analyte ions was evaluated. The results obtained are presented in Fig. 3. The anionic surfactant, SDS, is effectively sorbed on the positively charged alumina surfaces in acidic solution, forming aggregates termed as hemi micelles and ad-micelles (Stafiej and Pyrzynska, 2008), which present high potential as the sorbent materials for SPE. In the absence of SDS, ions were not retained on SDS-alumina. Therefore, the addition of SDS is necessary.

Amount of SDS on recovery of metal ions (N = 3).
Figure 3
Amount of SDS on recovery of metal ions (N = 3).

The retention of the metal ions was examined in relation to the amount of surfactant, which was varied from 30.0 to 80.0 mg. It was found that the recoveries of lead and silver were gradually increased up to 70.0 mg of the SDS. Therefore, 70.0 mg of the SDS was used for lead and silver.

3.4

3.4 Effect of Alizarin red-s amount

In order to determine the amounts of ligand required for quantitative recoveries for Pb2+ and Ag+ ions, the proposed method was applied. Changing ligands amount to the range of 20.0–60.0 mg. The recovery values of the analyte metal ions (Fig. 4) increased with increasing amounts of ligand added and reached quantitative values of 98.0% with 50.0 mg of ligand. Therefore, this value was recommended as an optimum ligand value for quantitative recovery.

Effect of Alizarin red-s amount on recovery of metal ions (N = 3).
Figure 4
Effect of Alizarin red-s amount on recovery of metal ions (N = 3).

3.5

3.5 Choice of the eluent

The other important factors that affect the preconcentration procedure is the type, volume and concentration of the eluent used for the removal of metal ions from the sorbent. Optimization of the elution conditions was performed in order to obtain the maximum recovery with the minimal concentration and volume of the elution solution. The different concentrations and volumes of nitric acid, acetic acid, phosphoric acid and sulfuric acid were tested to remove the bound metal ions from the sorbent, 5.0 mL of 4.0 mol L−1 H3PO4 solution was found to be satisfactory (recovery >99.0%) for lead and silver and the results are shown in Table 2.

Table 2 Effect of type and concentration of eluting agent on recovery of analytes.
Condition of eluting agent Recovery (%)
Pb(II) Ag(I)
1.0 mol L−1 CH3COOH 51.5 ± 0.6 59.4 ± 1.0
1.0 mol L−1 HNO3 70.1 ± 0.5 71.3 ± 0.8
2.0 mol L−1 H2SO4 66.5 ± 0.3 63.4 ± 0.9
0.5 mol L−1 EDTA 54.1 ± 1.1 55.9 ± 1.1
2.0 mol L−1 H3PO4 73.7 ± 1.0 71.4 ± 0.9
3.0 mol L−1 H3PO4 82.5 ± 0.5 84.6 ± 0.8
4.0 mol L−1 H3PO4 99.2 ± 0.6 99.7 ± 0.9
5.0 mol L−1 H3PO4 99.1 ± 1.0 99.5 ± 1.0

3.6

3.6 Adsorption capacity

The sorption capacity is an important factor because it determines how much sorbent is required for quantitative enrichment of the analyte from a given solution (Tunceli and Turker, 2002). In order to determine this, 100.0–5000.0 μg of analytes was loaded to the column containing 150.0 mg of modified solid phase and recoveries were investigated. Then, Langmuir isotherms were plotted in order to determine the adsorbent capacity. This isotherm is one of the most well known and applied adsorption isotherms and described by the following equation:

(A.1)
q e = q max a L C e / 1 + a L C e where qe is the amount of metal adsorbed per unit weight of the adsorbent (mg g−1) at equilibrium, Ce the final concentration in the solution (mg L−1), qmax the maximum adsorption at monolayer coverage (mg g−1), and aL the adsorption equilibrium constant that is related to energy of adsorption (L mg−1). The equation given above can be rearranged as follows:
(A.2)
C e / q e = C e / q max + 1 / a L q max A plot of Ce/qe versus Ce shows linearity; hence Langmuir constants qmax and aL can be calculated from the gradient and intercept of the plot, respectively (Fig. 5) (Tan and Xiao, 2009).
Langmuir isotherms for determination of the solid-phase capacities.
Figure 5
Langmuir isotherms for determination of the solid-phase capacities.

3.7

3.7 Interference investigation

The effect of different cations and anions was also examined. In order to assess the possible analytical applications of the recommended procedure, the interference of several cations and anions were examined under optimized conditions. For these studies an aliquot of aqueous solution (50.0 mL) containing 5.0 μg of analyte ions was taken with different amounts of foreign ions and the procedure was implemented. The tolerance limit was defined as the highest amount of foreign ions that produced an error no greater than ±3.0% in the determination of investigated analyte ions. The results are summarized in Table 3. It can be seen that a good selectivity is achieved.

Table 3 Effect of foreign ions on percent recovery of lead and silver ions (N = 3).
Diversions Fold ratio ion/analyte Recovery (%)
Pb(II) Ag(I)
Ni2+ 600 96.0 ± 1.0 95.5 ± 2.0
Mg2+ 1000 97.0 ± 1.0 98.0 ± 1.0
Co2+ 500 96.0 ± 1.0 99.5 ± 2.0
Na+ 800 98.0 ± 1.0 97.0 ± 2.0
K+ 800 98.0 ± 1.0 98.0 ± 1.0
Li+ 800 97.0 ± 2.0 98.0 ± 1.0
Ba2+ 1000 98.0 ± 1.0 97.0 ± 1.0
Mn2+ 600 96.0 ± 1.0 99.3 ± 1.0
Cd2+ 600 95.0 ± 1.0 98.8 ± 1.0
Se4+ 1000 99.5 ± 1.0 99.5 ± 3.0
Cl– 400 97.0 ± 2.0 98.0 ± 2.0
NO 3 - 700 97.0 ± 1.0 97.0 ± 1.0
SO 4 2 - 800 98.0 ± 1.0 98.0 ± 1.0

3.8

3.8 Effect of the sample rate

The percent sorption of lead and silver ions on sorbent surfaces as a function of sample solution flow rate was examined in the range of 0.5–6.0 mL min−1. The results indicated that at flow rates greater than 2.0 mL min−1 there was a decrease in the recovery of lead and silver. The reason for this decrease is probably due to the insufficient contact of the metal ions and the absorbent to reach equilibration. Thus, a flow rate of 2.0 mL min−1 was chosen for studies.

3.9

3.9 Investigation of preconcentration factor and loading capacity

The elution volume strongly affects the preconcentration factor, defined as the ratio of sample volume to elution volume. By applying the optimum condition volumes up to 500.0 mL of 1.0 μg L−1 of lead and silver can be completely adsorbed on the column and could be easily desorbed (by 5.0 mL of H3PO4 solution) and detected by FAAS. This shows that a preconcentration factor of 100.0 is achievable by the system.

The capacity of immobilized Alizarin on surfactant coated alumina on sorption of lead and silver were examined and found to be 2.3 and 2.1 mg g−1 of solid phase, respectively. This indicates that the column is capable of absorbing large amounts of lead and silver.

3.10

3.10 Characteristics of the method

Under the specified experimental conditions the calibration curves for lead and silver were linear from 100.0 to 1250.0 and 140.0 to 2950.0 μg L−1 with a correlation coefficient of 0.9989 and 0.9979, respectively. RSD values for slope and intercept for Pb(II) were 1.6 and 2.5 and for Ag(I) were 2.4 and 1.9, respectively.

The LOD obtained from C = Kb Sb m−1 for a numerical factor Kb = 3.0 for lead and silver were 18.0 and 55.0 μg L−1 respectively. The characteristics of the proposed method are shown in Table 4.

Table 4 Analytical characteristics of presented method.
Analytical parameter Pb(II) Ag(I)
Linear range (μg L−1) 100.0–1250.0 140.0–2950.0
Regressions equation (C: μg L−1) A = 6 × 10−4CPb(II) + 0.0424 A = 1 × 10−4CAg(I) + 0.0277
R2 0.9982 0.9997
Limit of detectiona (μg L−1) 18.0 55.0
R.S.D. (%) (n = 6) 1.8 (C = 300.0 μg L−1) 2.1 (C = 200.0 μg L−1)
a Determined as 3 SB/m (where SB and m are the standard deviation of the blank signal and the slope of the calibration graph, respectively).

3.11

3.11 Application of proposed method for the determination of trace analytes

In order to check the applicability of the proposed method in various real samples, lead and silver which were determined in an environment such as soil, waste water, water and amalgam and biological samples such as blood, mushroom and hair were adjusted to the optimum pH and subjected to the recommended column procedure for the preconcentration and determination of metal ions. The precision values, RSDs for replicates of one extract, repeatability (intra-assays precision) and reproducibility (inter-assay precision) are reported in Tables 5 and 6. The results reported in Tables 5 and 6 show that the proposed method is suitable for the determination of lead and silver ions in real samples.

Table 5 Determination of Pb and Ag in soil and water samples.
Samples Metal ions Added (μg L−1) Found (μg L−1) R.S.D. (%) Recovery (%)
Extracta
Pb(II) 0 135.0 1.9 –
Soil 300.0 434.0 1.9 99.7
Ag(I) 0 145.0 1.5 –
150.0 295.3 1.7 100.2
River waterb Pb(II) 0 NDc – –
300.0 300.0 1.8 100.0
Ag(I) 0 ND – –
150.0 150.0 1.0 100.0
Wastewaterd Pb(II) 0 180.0 1.5 –
300.0 479.2 1.8 99.7
Ag(I) 0 300.0 1.9 –
150.0 449.4 1.0 99.6
Repeatabilitye
Pb(II) 0 134.1 1.8 –
Soil 300.0 432.0 2.1 99.3
Ag(I) 0 142.0 2.5 –
150.0 293.3 2.1 100.9
River water Pb(II) 0 NDc – –
300.0 294.0 1.9 98.0
Ag(I) 0 ND – –
150.0 152.1 3.0 101.4
Wastewater Pb(II) 0 180.0 2.5 –
300.0 480.2 3.2 100.1
Ag(I) 0 297.4 1.9 –
150.0 446.3 1.8 99.3
Reproducibilityf
Pb(II) 0 133.8 2.7 –
Soil 300.0 438.2 3.2 101.5
Ag(I) 0 142.0 2.6 –
150.0 289.3 2.7 98.2
River water Pb(II) 0 NDc – –
300.0 302.0 2.3 100.6
Ag(I) 0 ND – –
150.0 152.9 1.8 101.9
Wastewater Pb(II) 0 178.1 2.5 –
300.0 476.8 3.2 99.6
Ag(I) 0 301.3 2.9 –
150.0 452.1 3.0 100.5
a Relative standard deviations (RSD) for four replicates of one extract.
b River water sample was collected from of Kor River Marvdasht, Iran.
c Not Detect.
d Wastewater sample was collected from of Shiraz Industrial State, Iran.
e Repeatability n = 3.
f Reproducibility n = 6.
Table 6 Determination of Pb and Ag in some real samples.
Samples Metal ions Added (μg L−1) Found (μg L−1) R.S.D. (%) Recovery (%)
Extracta
Pb(II) 0 130.0 1.3 –
Hair 300.0 429 1.5 99.7
Ag(I) 0 NDb – –
150.0 150.0 1.0 100.0
Pb(II) 0 130.0 1.3 –
Blood 300.0 430.8 1.5 100.3
Ag(I) 0 145.0 1.5 –
150.0 296.1 1.7 100.7
Pb(II) 0 140.0 2.3 –
Mushroom 300.0 438.2 1.5 99.4
Ag(I) 0 ND – –
150.0 151.8 1.5 101.2
Pb(II) 0 ND – –
Amalgam 300.0 300.0 1.5 100.0
Ag(I) 0 190.0 1.7 –
150.0 340.0 1.5 100.0
Repeatabilityc
Pb(II) 0 128.4 2.3 –
Hair 300.0 429.5 2.9 100.4
Ag(I) 0 ND – –
150.0 152.3 2.0 101.5
Pb(II) 0 129.5 3.3 –
Blood 300.0 434.8 2.2 101.8
Ag(I) 0 147.0 2.5 –
150.0 298.6 1.7 101.1
Pb(II) 0 142.3 – –
Mushroom 300.0 442.2 2.1 99.9
Ag(I) 0 ND - -
150.0 149.7 2.4 99.8
Pb(II) 0 ND – –
Amalgam 300.0 289.2 1.1 96.4
Ag(I) 0 188.4 2.8 –
150.0 343.2 1.5 103.2
Reproducibilityd
Pb(II) 0 128.3 2.8 –
Hair 300.0 426.7 2.5 99.5
Ag(I) 0 ND – –
150.0 146.5 2.9 97.7
Pb(II) 0 126.7 3.2 –
Blood 300.0 423.8 3.4 99.0
Ag(I) 0 141.3 1.9 –
150.0 293.1 2.2 101.2
Pb(II) 0 136.5 – –
Mushroom 300.0 435.2 3.4 99.6
Ag(I) 0 ND – –
150.0 147.1 2.5 98.1
Pb(II) 0 ND – –
Amalgam 300.0 287.3 2.4 95.8
Ag(I) 0 185.4 3.1 –
150.0 331.3 2.6 97.3
a Relative standard deviations (RSD) for four replicates of one extract.
b Not detect.
c Repeatability n = 3.
d Reproducibility n = 6.

4

4 Conclusion

The proposed procedure provides a simple, sensitive, precise, reliable and accurate technique for the preconcentration and determination of lead and silver. The important features of the proposed method are its higher adsorption capacity and good preconcentration factor. The developed method is sensitive in detecting lead and silver at μg L−1 levels. Comparative data from some recent studies on solid phase extraction studies are given in Table 7.

Table 7 Comparative data from some recent studies for preconcentration of trace metals.
Chelating agent/solid phase adsorbent Method Preconcentration factor References
1,5-diphenyl carbazone/Amberlite XAD-16 AAS 25.0 Tunceli and Turker (2002)
DuoliteGT-73 resin ICP-AES 40.0 Pohl and Pruiszz (2004)
Dithioacetal/SiO2 CV-AAS 5.0 Mahmoud and Gohar (2000)
Bis(2-mercaptophenyl)ethanediamide/silica gel Spectrophotometry 50.0 Kera and Tekin (2005)
Dithizone/Chromosorb-108 AAS 71.0 Tuzen and Soylak (2006)
HgI 4 2 - -Aliquat-336/naphthalene Anodic stripping voltammetry 80.0 Pourrezza and Behpour (2003)
Alizarin red-s γ-alumina FAAS 100.0 In this work

Acknowledgments

The authors gratefully acknowledge the support of this work by Shiraz Payame Noor University Research council (Grant No. D/7/69604).

References

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