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Food and Chemical Toxicology 49 (2011) 12421248

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Food and Chemical Toxicology


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Determination of some heavy metals in food and environmental samples by ame atomic absorption spectrometry after coprecipitation
Mustafa Soylak , Ayse Aydin
University of Erciyes, Faculty of Science, Chemistry Dept., 38039 Kayseri, Turkey

a r t i c l e

i n f o

a b s t r a c t
A novel preconcentration procedure based coprecipitation of Cu(II), Co(II), Cd(II), Ni(II), Mn(II), Fe(III) and Pb(II) on thulium hydroxide precipitate has been presented prior to ame atomic absorption spectrometric determination of them in environmental samples. The analytical parameters that inuenced the quantitative coprecipitation of analytes including amount of thulium, pH, duration time, etc. were investigated. The effects of alkali, earth alkali, and some transition metals on the recoveries were also studied. Under the optimized conditions, the detection limits (3 sigma, N = 10) for the analytes were in the range of 0.11.6 lg/L, respectively. The validation of the presented coprecipitation method was checked by the analysis of certied reference materials (TMDA 54.4 fortied lake water and HR-1 Humber river sediment). The proposed coprecipitation method has been successfully applied for the determination of traces of copper, cobalt, cadmium, nickel, manganese, iron and lead in food and environmental samples. 2011 Elsevier Ltd. All rights reserved.

Article history: Received 16 November 2010 Accepted 2 March 2011 Available online 16 March 2011 Keywords: Coprecipitation Food Heavy metal Preconcentration Atomic absorption spectrometry

1. Introduction Heavy metal levels in food and environmental samples are an important key for the environmental pollution (Cayir and Coskun, 2010; Ieggli et al., 2010; Grabarczyk and Korolczuk, 2010; Kolachi et al., 2010a,b; Afkhami et al., 2011). The sources of them are generally industry and trafc (Khadro et al., 2009; Biyik and Tapramaz, 2009; An et al., 2009; Kazi et al., 2010; Soylak et al., 1996). Their accurate determinations in environmental samples are main eld in analytical chemistry (Soylak et al., 1999; Narin et al., 2001; Shokrollahi et al., 2009; Depecker et al., 2009; Ozeroglu and Keceli, 2009; Ciftci, 2010). High levels of matrix components are inuenced determinations of heavy metal ions. In order to remove matrix components from the traces heavy metals, separation methods like solid phase extraction, cloud point extraction, solvent extraction, etc. have been widely used (Soylak et al., 1993; Derakhshi et al., 2009; Karve and Rajgor, 2009; Burham, 2009; Celik et al., 2010; He et al., 2010; Khan et al., 2009; Ghaedi et al., 2009; Zhang et al., 2010). Another important advantage of usage of separation methods is improvements in the limit of detection of the analytes, due to lower nal volumes (Ghaedi et al., 2007; Kazi et al., 2009; Khan et al., 2010; Abulhassani et al., 2010; Panahi, 2009; Sahin et al., 2010; Ghaedi and Niknam, 2010; Yalcinkaya et al., 2010; Islam et al., 2010). Coprecipitation is also widely applied for separation and preconcentration of analytes from a liquid matrix and/or puried ex Corresponding author. Tel./fax: +90 352 4374933.
E-mail addresses: msoylak@gmail.com, soylak@erciyes.edu.tr (M. Soylak). 0278-6915/$ - see front matter 2011 Elsevier Ltd. All rights reserved. doi:10.1016/j.fct.2011.03.002

tracts for heavy metal ions (Aydin and Soylak, 2007; Samaci and Kartal, 2010; Frigge and Jackwerth, 1991; Majewski and Cyganski 1982; Soylak et al., 2005; Saracoglu et al., 2001; Chen et al., 1997). Coprecipitation has some advantages: simple, rapid and analytes could be preconcentrated and separated from the matrix simultaneously. Inorganic and organic coprecipitants have been used successfully in the coprecipitation of heavy metal ions at trace levels. Hydroxides of various metal ions as coprecipitant have been used for the preconcentration and separation of some heavy metals in literature. Thulium hydroxide precipitate (Aydin and Soylak, 2009) has been used for the speciation and preconcentration of chromium species. According to our literature survey, there is not any work for the usage of thulium hydroxide precipitate for the preconcentration of traces heavy metal ions except this work. The aim of the presented work is to show the possibility of the usage of thulium hydroxide precipitate for the quantitative coprecipitation of traces of Cu(II), Co(II), Cd(II), Ni(II), Mn(II), Fe(III) and Pb(II) and to application of the procedure prior to their ame atomic absorption spectrometric determination of them in environmental samples including some foods. 2. Experimental 2.1. Instruments A PerkinElmer Model 3110 atomic absorption spectrometer equipped with PerkinElmer single-element hollow cathode lamps and a 10-cm airacetylene burner were used for the determination of the metal ions. All instrumental settings were those recom-

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mended in the manufacturers manual book that are given in Table 1 A pH meter, Sartorius PT-10 Model glass-electrode was employed for measuring pH values in the aqueous phase. ALC PK 120 model centrifuge was used to centrifuge of solutions. The water was puried in a Human model RO 180, resulting water with a conductivity of 1 lS/cm.

2.2. Reagents All the reagents used were of analytical grade. Laboratory glassware was kept overnight in a 10% v/v HNO3 solution and then rinsed with deionized double distilled water. 0.1% w/v thulium (III) solution was prepared freshly by dissolving Tm2O3 (Fluka, Buchs, Switzerland) in small amounts of 1 M HNO3 and diluting to 100 ml with double distilled water. It was prepared daily. NaOH solution (1 M) was used at the pH adjustments. Stock standard solutions of analytes, 1000 mg/L, was prepared by dissolving

appropriate amount of nitrate salts of analytes in 1% nitric acid (Merck, Darmstadt, Germany). Stock metal ion solutions were diluted daily for obtaining reference and working solutions. The calibration curve was established using the standard solutions prepared in 1 mol/L HNO3 by dilution from stock solutions. TMDA 54.4 fortied lake water and HR-1 Humber river sediment certied standard reference materials were supplied by National Water Research Institute, Environment Canada (Burlington, ON, Canada). 2.3. Recommended procedure One milliter of 0.1% (1 mg) thulium(III) was added to 25 mL of solution containing 1020 lg analyte ions. Then the pH of the solution was adjusted to related pH by the addition of 1 mol/L NaOH. The tube is slowly and carefully shaked for several seconds and allowed to stand for 15 min. Then, the solution was centrifuged at 3500 rpm for 15 min. The supernatant was removed. The precipitate remained adhering to the tube was dissolved with 0.5 mL of concentrated HNO3. The volume was completed to 5.0 mL by the addition of distilled water. The number of replicates for the test workings was three. The levels of analyte ions were determined by ame atomic absorption spectrometry. 2.4. Applications 0.25 g of HR-1 Humber river sediment certied reference material or 1.0 g of soil sample or 1.0 g food sample was digested with

Table 1 Instrumental conditions for ame atomic absorption spectrometer. Element Fe Pb Ni Co Cd Cu Wavelength (nm) 248.3 283.3 232.0 240.7 228.8 324.8 Slit width (nm) 0.2 0.7 0.2 0.2 0.7 0.7 Lamp current (mA) 30 15 30 30 12 15

Fig. 1. The effects of pH on the coprecipitation efciencies of analyte ions (N = 3).

Fig. 2. Inuences of thulium(III) as carrier element on the recoveries of analyte ions by the presented work (N = 3).

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Table 2 Effects of duration time for thulium hydroxide precipitate for the recoveries of the analytes (N = 3). Recovery (%) Time (min) 0 5 10 15 20 25 30 Cu 86 1 93 2 98 0 99 1 99 2 99 1 99 1 Co 84 1 94 2 96 2 99 1 100 1 100 0 98 1 Ni 73 3 83 2 92 1 96 2 97 1 100 0 96 2 Fe 84 1 87 1 91 2 95 1 99 1 98 1 96 2 Cd 86 1 93 0 95 1 96 0 99 2 99 1 97 1 Pb 84 2 88 1 99 0 99 0 100 1 100 1 97 2

to 20 mL with distilled water. Then the procedure given in Section 2.3 was applied. Analyte elements in nal solution were determined with ame AAS. The proposed method was applied to TMDA 54.4 fortied lake water. The pH of the samples was adjusted to 11. Then the preconcentration procedure as given above was applied to understudy water samples. The analyte concentrations in the last solution were determined by ame atomic absorption spectrometry (FAAS).

3. Results and discussion 3.1. Effects of pH on the recoveries of analytes

Table 3 Inuences of the centrifugation time on the recoveries of the analytes (N = 3). Recovery (%) Time (min) 5 10 15 20 25 30 Cu 88 1 93 1 98 2 99 2 99 1 99 1 Co 86 2 90 1 96 1 97 2 100 1 98 1 Ni 81 2 87 3 95 2 96 1 98 1 98 1 Fe 87 2 92 2 97 1 98 1 100 2 99 1 Cd 80 1 85 2 96 1 99 1 99 1 99 1 Pb 84 2 91 2 98 1 100 1 99 1 99 1

The inuences of pH on the recoveries of analyte ions were investigated in the pH range of 712. The pH adjustments of the model solutions were performed by the addition of 1 M NaOH. The results are given in Fig. 1. At the pH range of 1012, all the analyte ions were simultaneously and quantitatively (>95%) recovered. All further works were performed at pH 11.

3.2. Inuences of amounts of thullium(III) as carrier element The inuences of amounts of thulium(III) as carrier element on the recoveries of Cu(II), Co(II), Cd(II), Ni(II), Mn(II), Fe(III) and Pb(II) ions were also examined by using model solutions at pH 11 with other parameters kept constant. The results are depicted in Fig. 2. The recoveries of analyte ions were below 60% without thulium(III). The quantitative recoveries were obtained for analyte ions at the thullium(III) amounts range of 1.03.0 mg (Fig. 2). All further works were carried out by the addition of 1.0 mg of thulium(III) as carrier element.

Table 4 The effects of centrifugation speed on the recoveries of analytes (N = 3). Recovery (%) Speed (rpm) 1000 1500 2000 2500 3000 3500 4000 Cu 89 1 93 1 95 1 97 2 98 2 100 0 100 0 Co 84 1 86 1 90 1 92 2 98 2 100 1 100 1 Ni 74 2 78 2 88 1 94 1 100 2 100 1 100 1 Fe 84 1 86 1 86 1 94 1 97 1 100 1 98 1 Cd 78 2 80 2 91 1 92 2 95 1 97 1 99 1 Pb 80 2 82 2 83 2 85 1 97 1 98 1 100 1

3.3. Effects of duration time The inuences of duration time for the coprecipitation on the recoveries of analyte ions were also studies in the time range of 030 min. The results are summarized in Table 2. Quantitative recoveries for all the analytes were obtained after 15 min of duration time. The further studies were performed at 15 min of duration time.

16 mL aqua regia at 95 C. The mixture was evaporated almost to dryness and mixed with 8 mL of aqua regia. Then it was again evaporated to dryness. After evaporation 89 mL of distilled water was added and the sample was mixed. The resulting mixture was ltered through a blue band lter paper. The ltrate was diluted

Fig. 3. Relation between sample volume and recoveries of analytes (N = 3).

M. Soylak, A. Aydin / Food and Chemical Toxicology 49 (2011) 12421248 Table 5 Matrix effects (N = 3). Ion Concentration (mg/L) Added As Recovery (%) Pb Na+ Ca2+ K+ ClSO42PO43Zn2+ Mn2+ Cr3+ Mg2+ Pb2+ Cu2+ Ni2+ Co2+ Fe3+ Cd2+ 20,000 5000 5000 20,000 3000 3000 40 10 20 1250 20 20 20 20 20 50 NaNO3 CaCl2 KNO3 NaCl Na2SO4 Na3PO4 Zn(NO3)2 MnSO4H2O Cr(NO3)39H2O Mg(NO3)2 Pb(NO3)2 Cu(NO3)23H2O Ni(NO3)26H2O Co(NO3)26H2O Fe(NO3)39H2O Cd(NO3)2 100 1 98 1 98 1 100 1 99 1 98 2 98 1 100 1 100 1 98 1 98 1 100 1 98 1 97 1 99 1 Cu 96 1 100 1 100 1 96 1 99 0 99 1 96 2 98 2 99 1 99 1 98 2 97 1 99 0 100 1 100 0 Ni 99 1 100 1 100 1 98 1 97 2 97 1 100 0 100 0 100 0 99 1 100 1 99 1 102 1 100 1 100 1 Co 100 1 100 1 101 2 101 2 100 1 100 0 100 1 100 1 98 1 100 2 98 1 100 0 100 0 100 0 99 1 Fe 101 1 100 1 96 1 99 1 100 0 96 2 100 1 99 1 98 1 96 2 98 1 96 2 95 2 100 0 99 1 Cd

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98 2 99 2 98 2 98 2 98 1 97 1 101 1 100 0 99 1 97 1 99 1 98 1 100 1 99 2 98 1

Table 6 Detection limits for analytes by the presented coprecipitation procedure (N = 10). Analyte Cu Pb Ni Fe Cd Co Detection limits (lg/L) 0.51 1.60 1.41 0.50 0.10 0.50

Table 8 Application of the presented procedure for a tap water sample (N = 3). Analyte Pb Added (lg/L) 0 5 10 20 40 0 5 10 20 40 0 5 10 20 40 0 5 10 20 40 0 5 10 20 40 0 5 10 20 40 Found (lg/L) BDLa 5.2 0.6 10.0 1.0 19.1 0.6 38.6 0.6 BDL 4.9 0.6 10.2 0.6 20.0 1.0 38.0 1.0 2.7 0.6 5.2 0.6 10.0 1.0 20.0 1.0 39.0 1.0 BDL 5.0 0 9.8 0.6 20.0 1.0 39.0 1.0 BDL 5.0 0 9.8 0.6 19.0 1.0 40.0 1.0 BDL 4.8 0.6 9.6 0.6 19.6 0.6 39.3 0.6 Recovery (%) 104 100 96 97 99 103 103 97 105 100 101 99 100 98 100 98 100 98 98 102 98 97 98 99

Cu

3.4. Inuences of centrifugation time and centrifugation speed


Fe

The inuences of centrifugation time on the recoveries of analyte ions were investigated in the range of 530 min. The results are summarized in Table 3. The quantitative recoveries for Cu(II), Co(II), Cd(II), Ni(II), Mn(II), Fe(III) and Pb(II) ions were obtained after 15 min of centrifugation time. All further works were carried out at 15 min of centrifugation time. The effects of centrifugation speed on the recoveries of analytes were also studies on the presented thulium hydroxide coprecipitation system. The results are given in Table 4. The recoveries were quantitative for all analyte ions after 3000 rpm. Three thousand and ve hundred revolutions per minute was selected as optimal centrifugation speed. 3.5. Sample volume and preconcentration factor The effect of the sample volume on the recoveries of analyte ions was investigated in the sample volume range of 20750 mL by using model solutions. The results are depicted in Fig. 3. Analyte ions were quantitatively (95%) recovered in the sample volume

Cd

Co

Ni

BDL: below the limit of detection.

Table 7 The results for reference standard materials. Analyte TMDA 54.4 fortied lake water (lg/L) Certied value Cu Cd Pb Ni Co
a

HR-1 Humber River Sediment (lg/g) Found value 443 1a 158 0 513 1 337 1 308 1 Certied value 78.5 4.30 144 38.5 13.0 Found value 78.2 0.6 4.2 0.1 143 1 38.0 1.0 12.4 0.6

443 158 514 337 309

mean standard deviation.

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Table 9 Application of the presented procedure for mint sample (N = 3). Analyte Pb Added (lg/L) 0 5 10 20 40 0 5 10 20 40 0 5 10 20 40 0 5 10 20 40 0 5 10 20 40 0 5 10 20 40 Found (lg/L) 2.2 0.6 6.8 0 12.4 1.0 22.0 0.6 43.0 0.6 5.3 0.6 10.0 0 15.2 1.0 25.4 1.0 45.5 1.0 32.8 0.6 38.0 1.0 43.0 0.6 52.4 0 73.3 0.6 BDL a 4.8 0 10.2 0.6 19.3 1 39.4 1 BDL 4.8 0 9.5 0 19.8 0 39.8 0 1.8 0.6 6.5 0 12.0 0.6 21.5 0.6 40.2 0 Recovery (%) 92 102 99 102 94 99 100 100 104 102 101 100 96 102 97 99 96 95 99 99 95 102 98 96

bance alteration. The ions do not interfere under the experimental conditions used. Some transition metals at mg/L levels were not interfered on the recoveries of the analytes. 3.7. Analytical features The limits of detection (LOD) of the proposed procedure for the determination of analyte elements were studied under the optimal experimental conditions. The detection limits, dened as the concentration equivalent to 3 times the standard deviation of blank (N = 10, XL = (Xb + 3s)/PF, XL: limit of detection, Xb: blank value, PF: preconcentration factor) of the reagent blank (Madrakian et al., 2010; Kalfa et al., 2009; Soylak et al., 2010; Yildiz et al., 2011), are given in Table 6. The validation of the presented procedure is performed by the analysis of two certied reference materials (TMDA 54.4 fortied lake water and HR-1 Humber river sediment) for analytes. The certied and observed values for certied reference materials are given in Table 7. The results found were in good agreement with the certied values of CRMs. The recoveries of analytes spiked into a water samples and a mint sample were also studied, satisfactory results were obtained as shown in Table 8 for a tap water sample and in Table 9 for a mint sample. The recovery values calculated for the standard additions for the investigated analyte ions were always higher than 95%, thus conrming the accuracy of the procedure and the absence of matrix effects. 3.8. Applications Based on the above ndings, the presented procedure was applied to the determination of analytes in some real samples. The results are summarized in Table 10. The concentrations given in Table 10 for analytes have been calculated on the assumption of 100% recovery of the analyte ions.

Cu

Fe

Cd

Co

Ni

BDL: below the limit of detection.

range of 20600 mL. After 600 ml, the recoveries were decreased. A preconcentration factor of 120 for the analytes can be achieved when the nal volume was 5.0 mL.

3.6. Effect of matrix ions Alkali, earth alkali ions and anions at mg/l and higher levels are interferic effects on the determinations of heavy metal ions by ame atomic absorption spectrometry (Soylak, 2004; Sahan and Sahin, 2010; Sabermahani and Taher, 2010; Ghazy et al., 2010; Ahmed et al., 2010; Andal and Sakthi, 2010; Madrakian et al., 2010; Ghaedi et al., 2010; Marahel et al., 2011). The effects of these ion on the coprecipitation efciency of Cu(II), Co(II), Cd(II), Ni(II), Mn(II), Fe(III) and Pb(II) ions were examined by adding known concentrations of different ions. Then the coprecipitation procedure was applied all the diverse ions separately. The results are summarized in Table 5. The tolerated amounts of each diverse ion were the concentration values tested that caused less than 5% the absor-

4. Conclusion The presented procedure based on coprecipitation of some toxic metals by using thulium hydroxide precipitate is simple and accurate. The effects of matrix ions for AAS are tolerable. The recoveries of analyte ions on were greater than 95% at the optimal working conditions. The achieved detection limits of analyte are superior to some preconcentration/separation methods (Sabermahani and Taher, 2010; Ghazy et al., 2010; Ahmed et al., 2010; Andal and Sakthi, 2010; Madrakian et al., 2010). The proposed method was also free of interference compared to conventional procedures to determine analyte metal ions. The presented coprecipitation method can be applied not only to water and food samples but also to geological samples.

Table 10 Determination of analytes in some real samples after application of proposed coprecipitation procedure (N = 3). Concentration (lg/g) Sample Clove Black tea Mint Ginger Nettle Soil from Nevsehir Soil sample from a gold mine in Izmir
a

Pb BDL 2.5 0.1 6.0 0 5.7 0.6 2.6 0.7 61 2 53 2

Cu BDL 25 2 5.3 0.6 BDL BDL 135 2 94 1

Fe 33 1 a 81 1 12.8 0.6 14.2 0.6 18.0 0.6 620 2 570 3

Ni BDL 5.4 0.6 4.8 0.2 2.9 0.1 BDL 82 1 47 1

Cd BDL BDL BDL BDL BDL 19 1 12 1

Co BDL 3.0 1.0 BDL BDL BDL 23 1 19 1

Cr BDL 3.0 0.6 BDL BDL BDL 95 2 63 1

BDL: below the limit of detection.

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Conict of Interest The authors declare that there are no conicts of interest. Acknowledgment The authors are grateful for the nancial support of the Unit of the Scientic Research Project of Erciyes University (Project No.: FBY-10-3028). References
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