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/lp/springer-journals/mucor-pusillus-immobilized-amberlite-xad-4-biocomposites-for-QSnGBnsKwX
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- Springer Journals
- Copyright
- 2018 The Author(s).
- eISSN
- 2093-3371
- DOI
- 10.1186/s40543-018-0141-5
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Abstract
Background: Solid phase extraction has been an effective tool for the determination of metal ions at trace or sub trace level from environmental aquatic streams. Sensitivity, accuracy, versatility and reusability of adsorbent entitle the solid phase as effective technique for the determination of metal ions. Methods: A solid phase extraction procedure has been described for the determination of Cd, Cu, and Pb by High Resolution–Continuum Source Flame Atomic Absorption Spectrometry HR-CS FAAS using a mini-column of Mucor pusillus (Lindt., 1886) immobilized on Amberlite XAD-4. Method has been optimized by changing the pH of analyte solution, solid phase dosage, volume of eluents, flow rate of sample solution and volume of the sample solutions. Results: The recoveries of Cd, Cu, and Pb under the optimum conditions were 99±3%, 97±2% and 96±2%, respectively. The resulting preconcentration procedure ensured a 50-fold improvement in the sensitivity of the elements. The detections limits were 62, 74 and 235 ng/mL for Cd, Cu, and Pb before enrichment, respectively. The method was validated by analysis of tomato leaves reference materials (SRM 1573a). Conclusions: The proposed enrichment method has been successfully applied for the determination of Cd, Cu, and Pb in tomato leaves and water samples with a relative error ≤8%. This method is simple, sensitive, and accurate especially for water sample, only 200 mg of sorbent are required to capture the analytes. It can be concluded that the use of Mucor pusillus (Lindt., 1886) enhanced the sorption ability of Amberlite XAD-4 resin for the retention of Cd, Cu, and Pb. Keywords: Mucor pusillus, Amberlite XAD-4, Heavy metal, Preconcentration, Solid-phase extraction Background samples. These problems can be solved by applying Determination of metal ions in the environmental effective separation and preconcentration techniques samples at trace or sub trace levels has been a chal- for the quantification of metal ions up to the detec- lenging task for researchers. Analytical determination tion limits. Various methods have been discussed and needs specificity, sensitivity, accuracy, and versatility. applied for the preconcentration of metal ions, in- Many instrumental methods have been used to find cluding liquid-liquid extraction (LLE) (Anthemidis the direct determination of metal ions, but it seems and Ioannou 2009), coprecipitation (Saracoglu et al. impossible because of matrix interferences and low 2012), cloud point extraction (CPE) (Hongbo et al. concentration of metal ions in the environmental 2013), and solid-phase extraction (SPE) (Sahmetlioglu et al. 2014; Baytak and Arslan 2015;Baytak and * Correspondence: channa_abdulmajid@yahoo.com Kasumov 2017),which are used to solve these prob- Department of Chemical Engineering, Faculty of Engineering, Suleyman lems of trace metal determinations. SPE has been a Demirel University, 32260 Isparta, Turkey most promising technique because of its simplicity, Institute of Advanced Research Studies in Chemical Sciences, University of Sindh, Jamshoro, Pakistan use of small volume of solvent, and ability to obtain a Full list of author information is available at the end of the article © The Author(s). 2018 Open Access This article is distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made. Baytak et al. Journal of Analytical Science and Technology (2018) 9:9 Page 2 of 6 high preconcentration factor and high speed (Baytak of 1000 μg/mL Cd, Cu, and Pb (Specx Certiprep) in and Arslan 2015; Baytak and Kasumov 2017; 2% HNO . The working solutions were prepared by Krawczyk et al. 2014) .Various adsorbents have been dilution from the stock solution. Amberlite XAD-4 investigated in SPE such as multi-walled carbon nano- (Sigma Chem. 20–40 mesh, 780 m /g) was used as a tubes (Li et al. 2013;Alothmanetal. 2012;Wang et substrate for the immobilization of Mucor pusillus al. 2011), magnetic nanoparticles (Asgharinezhad et (Lindt., 1886). al. 2014;Khajeh 2009), solid sulfur (Parham et al. 2009), cotton (Faraji et al. 2009), modified porous ma- Preparation of solid phase terials (Matbouie et al. 2013;Taghizadehetal. 2013; Mucor pusillus (Lindt., 1886) was grown, prepared, and Pereira et al. 2010), and Amberlite XAD resins for immobilized according to the procedure given by Baytak preconcentration and separation of trace metal ions and Turker (2009). Two hundred milligrams of from various media (Baytak and Turker 2005a). Amberlite XAD-4 loaded with Mucor pusillus (Lindt., Chelating polymeric resin can be modified by im- 1886) was packed in a glass column (8 mm i.d and mobilizing suitable and selective ligands onto func- 200 mm length). Before using, 1 mol/L HCl solution and tionalized polymeric solid surfaces. Many chelates doubly distilled deionized water were passed through the have been suggested using Amberlite XAD polymer column in order to clean it. Then, the column was con- as a solid support because of higher adsorption cap- ditioned for the optimization of pH experiments. acity. Functionalized polymers having sound stability and higher affinity for the uptake of metal ions have Preconcentration procedure attracted the attention of researchers. Various ligands An aliquot of a solution (100 mL) containing 20 μg have been used to develop Amberlite XAD as a solid of Cd, 20 μgofCu,and20 μgofPb was taken, and support for the metal ions such as hydroxamic acid the pH was adjusted to the desired value with hydro- (Kumar et al. 2011), 2-amino-5-hydroxy benzoicacid chloric acid or ammonia. The resulting solution was (Sabarudin et al. 2007), 2, 6-diacetylpyridine (Karadas passed through the column by a flow rate adjusted to et al. 2011), and fluorinated β-diketone (Waqar et al. the desired value. The retained metal ions were then 2009). eluted from the solid phase with 10 mL of 1 mol/L Biosorption is a technique that is used to make HCl solution. This solution was aspirated into an air- complexes using biological materials with metal ions, acetylene flame for Cd(II), Cu(II), and Pb(II) determi- using their functional groups (Krishnani et al. 2008; nations by HR-CS FAAS. The Amberlite XAD-4 Pires et al. 2011). Recently, it has been investigated loaded with Mucor pusillus (Lindt., 1886) was used using various microbial biomasses for the preconcen- repeatedly after washing with 1 mol/L HCl solution tration of trace metals (Calero de Hoces et al. 2013; and distilled water, respectively. Baytak et al. 2011; Tuzen et al. 2008; Baytak and Turker 2005b; Baytak et al. 2014; Baytak and Turker Results and discussion 2009;Rajfuret al. 2010; Vilar et al. 2008) Effect of pH Microorganisms such as yeast (Baytak et al. 2011; The retention of Cd, Cu, and Pb metal ions on the solid Tuzen et al. 2008;Baytakand Turker 2005b), fungus phase was studied as a function of pH, amount of solid (Baytak et al. 2014; Baytak and Turker 2009), and phase, amount and type of elution solution, flow rate of algae (Rajfur et al. 2010; Vilar et al. 2008) have been sample solution, and volume of sample solution. The pH applied for the effective concentration of metal ions of Cd, Cu, and Pb ion solutions were optimized from 6 from the water system (Bakırcıoğlu et al. 2010;Wang to 8, while solid-phase dosage 200 mg, eluent 10 mL and Chen 2009). (1 M HCl), flow rate of sample solution 2 mL/min, and In the present study, a new method has been devel- sample volume 500 mL were kept constant. Maximum oped for the preconcentration of Cd, Cu, and Pb recovery was obtained at about pH 8 for all metal ions using Mucor pusillus (Lindt., 1886) immobilized as shown in Fig. 1. AmberliteXAD-4 as a solid phaseby HR-CS FAAS. Methods Effect of solid-phase dosage Apparatus and reagents The effect of solid-phase dosage was investigated in the An Analytical Jena model HR-CS FAAS was used for range 50–400 mg. It was found that the recoveries grad- the determination of the analytes. Doubly distilled ually increased up to 200 mg of solid phase and reached water and analytical reagent grade chemicals were plateau above 200 mg. Therefore, 200 mg of solid phase used. Cd, Cu, and Pb stock solutions (100 μg/mL) was found to be optimum for the preconcentration of all were prepared by dissolving the appropriate amounts metal ions. Baytak et al. Journal of Analytical Science and Technology (2018) 9:9 Page 3 of 6 Effect of flow rates of sample solutions The retention of metal ions on a solid phase depends upon the flow rate of sample solution. Flow rate was ex- amined under optimum conditions (pH, eluent type, dosage, and eluent volume). The solution was passed through the column with a flow rate adjusted in a range − 1 of 0.5–6 mL min . The optimum flow rate was found − 1 to be 3 mL min for all of the analytes. The flow rate − 1 of elution solution used was 3 mL min . Effect of the volume of sample solutions In order to determine the maximum applicable vol- ume of sample solution, the effect of change in the volume of sample solution passed through the col- umnonthe retentionofanalyteswas investigated; 50, 100, 250, 500, 750, and 1000 mL of sample solu- tions containing 20 μgofCd, Cu,and Pb were Fig. 1 Effects of pH on the recovery of Cd, Cu, and Pb, 0.2 μg/mL; passed through the column. It was found that all of solid phase, 200 mg; sample volume 500 mL; flow rate 3 mL/min; the metal ions up to 500 mL of sample solution elution solution 10 mL of 1 M HCI) could be recovered quantitatively. At higher sample volumes, the recoveries decreased gradually with in- creasing volume of sample solution. Because the elu- Effect of type and volume of elution solutions tion volume was taken 10 mL, a preconcentration In order to optimize the elution study, different elu- factor of 50 was obtained for all of the analytes. ents were used like HCl and HNO . Concentration 3 However, preconcentration factor with Agrobacter- and volume of these eluents were varied to investigate ium tumefaciens immobilized on Amberlite XAD-4 the effect of eluent type, volume, and concentration. has been reported 25. So, this method presents im- As a result of these experiments, 10 mL of 1 M HCl proved enrichment procedure with higher precon- solution was found to be satisfactory for these metals centration factor (Baytak and Turker 2005a). as shown in Table 1. Analytical performance of the method Under the optimum conditions, the precision of the method has been investigated. The recovery of the Table 1 Effect of the type, concentration, and volume of the analytes were found as 99 ± 3%, 97 ± 2%, and 96 ± 2% elution solution on the recovery of Cd, Cu, and Pb ions [sample for Cd, Cu, and Pb, respectively, with relative stand- volume, 50 mL; amount of the metals 10 μgofCd, Cu,and Pb;pH ard deviation lower than 2%. The accuracy of the 8for Cd,Cu, andPb] proposed method was checked by analyzing the certi- Element Type of Volume Concentration R% − 1 eluent (mL) (mmol mL ) fied reference material (SRM-1573a tomato leaves) (Table 2). The method was applied for the determin- Cd HCl 5 1 86 ation of Cd, Cu, and Pb in water and tomato leaves’ 10 1 99 samples. Results were shown in Tables 3 and 4. HNO 51 82 Method validation was confirmed by the good agree- 10 1 94 ment between the results of the proposed method Cu HCl 5 1 84 and certified values of Cd, Cu, and Pb. 10 1 97 Table 2 Determination of Cd, Cu, and Pb in (SRM-1573a tomato HNO 51 80 leaves) reference material 10 1 90 Element Certified (mg/kg) Found (mg/kg) Relative error, % Pb HCl 5 1 86 Cd 1.52 ± 0.04 1.45 ± 0.02 − 5 10 1 96 Cu 4.70 ± 0.14 4.52 ± 0.15 − 4 HNO 51 78 Pb 4.0 ± 0.1 3.72 ± 0.08 − 7 10 1 90 Pb was added to the solutions of SRM-1573a tomato leaves pffiffiffiffi a a Mean of three determinations Mean of five determinations at 95% confidence level (x±ts= N) Baytak et al. Journal of Analytical Science and Technology (2018) 9:9 Page 4 of 6 Table 3 Determination of Cd, Cu, and Pb in tomato leaves added to the synthetic samples containing Cd, Cu, and Pb. (0.5 g) Nitrate or chloride salts of interfering elements were a b Element Added (μg/g) Found (μg/g) Relative error, % added to the sample solutions. The concentration of ana- lytes was kept constant, and the concentration of interfer- Cd – N.D – − 1 ing ions was used in the range of 2–1000 μgmL .It can 10 9.4 ± 0.15 − 6 be seen in the Table 5 that there is no significant effect of Cu – 4.8 ± 0.1 – interfering ions on the recovery of analytes. 10 13.7 ± 0.3 − 7 Pb – N.D – 10 9.3 ± 0.2 − 7 Table 5 Effect of some ions on the recovery of Cd, Cu, and Pb [sample volume, 50 mL; amount of the metal ion, 10 μg; N.D not detected pffiffiffiffi Mean of five determinations at 95% confidence level (x±ts= N) pH 8] Shows the concentration of metal ions in tomato leaves and Kızılırmak river Interfering ion Interfering ion Recovery (R%) water samples concentration concentration Cd Cu Pb − 1 − 1 (μgmL ) (μgmL ) The effect of column reuse –– 99 97 96 The stability and potential recyclability of the column + Na 25 98 96 96 were assessed by monitoring the change in the recov- 50 98 96 95 eries of Cd, Cu, and Pb through several adsorption- 500 96 95 95 elution cycles. Each cycle was performed by passing 1000 95 94 93 50 mL of each analyte solution through the column and then stripping the analytes by appropriate eluent. K 25 98 97 96 The procedure was carried out ten times in a day, 50 98 97 96 and the next ten runs were made 1 day later, and so 500 96 96 95 on. The columns were stored in doubly distilled de- 1000 93 95 95 ionized water. The column seems to be relatively 2+ Mg 298 97 96 stable up to 40 for Cd and Cu and 35 runs for Pb. 597 97 94 This biomass seemed better than the other biomass reported earlier (Baytak and Turker 2005a). 10 94 93 92 2+ Ca 298 97 96 Effect of interfering elements 596 96 94 Interference study was carried out to examine the effect of 10 94 92 93 interfering ions; alkaline and alkaline earth elements were Co 5 98 97 96 10 97 97 96 Table 4 Determination of Cd, Cu, and Pb in tap water and 25 96 95 94 Kızılırmak river water samples (volume of samples 250 mL) a b Cr 5 98 97 96 Samples Element Added (μg/L) Found (μg/L) Relative error, % 10 97 96 95 Tap water Cd – N.D – 25 96 96 94 10 9.5 ± 0.2 − 5 Fe 5 98 97 96 Cu – 12.3 ± 0.4 – 10 97 97 95 10 20.6 ± 0.5 − 8 25 96 95 92 Pb – N.D – Mn 5 98 97 96 10 9.4 ± 0.3 − 6 10 97 97 95 River water Cd – N.D – 25 97 96 92 10 9.3 ± 0.3 − 7 Ni 5 98 97 96 Cu – 20.4 ± 0.6 – 10 97 96 95 10 28.7 ± 0.7 − 6 25 95 97 93 Pb – N.D – Zn 5 98 97 96 10 9.2 ± 0.2 − 8 10 97 96 94 N.D not detected pffiffiffiffi Mean of five determinations at 95% confidence level (x±ts= N) 25 96 95 92 Shows the concentration of metal ions in tomato leaves and Kızılırmak river water samples Mean of three determinations Baytak et al. Journal of Analytical Science and Technology (2018) 9:9 Page 5 of 6 Conclusions Baytak S, Mert R, Turker AR. Determination of Cu (II), Fe (III), Mn (II) and Zn (II) in various samples after preconcentration with Rhizopus oryzae loaded natural The proposed enrichment method has been successfully cellulose (almond bark). Intern J Environ Anal Chem. 2014;94:975–87. applied for the determination of Cd, Cu, and Pb in to- Baytak S, Turker AR. The use of agrobacterium tumefacients immobilized mato leaves and water samples with a relative error of ≤ on Amberlite XAD-4 as a new biosorbent for the column preconcentration of iron (III), cobalt (II), manganese (II) and chromium 8%. This method is simple, sensitive, and accurate espe- (III). Talanta. 2005a;65:938–45. cially for water sample; only 200 mg of sorbent are re- Baytak S, Turker AR. Determination of iron (III), cobalt (II) and chromium (III) in quired to capture the analytes. It can be concluded that various water samples by flame atomic absorption spectrometry after preconcentration by means of Saccharomyces Carlsbergensis immobilized on the use of Mucor pusillus (Lindt., 1886) enhanced the Amberlite XAD-4. Microchim Acta. 2005b;149:109–16. sorption ability of Amberlite XAD-4 resin for the reten- Baytak S, Turker AR. Determination of chromium, cadmium and manganese in tion of Cd, Cu, and Pb. By using bioadsorbent, higher water and fish samples after preconcentration using Penicillium digitatum immobilized on pumice stone. CLEAN- Soil Air Water. 2009;37:314–8. preconcentration factors have been obtained. Present Baytak S, Zereen F, Arslan Z. Preconcentration of trace elements from water study provides convenient and time-saving preconcen- samples on a minicolumn of yeast (Yamadazyma spartinae) immobilized TiO tration technique; only 30 min is required for recovery 2 nanoparticles for determination by ICP-AES. Talanta. 2011;84:319–23. Calero de Hoces M, Blazquez Garcia G, Ronda Galvez A. Biosorption of Cu2+ in a and regeneration of biosorbent. packed bed column by almond shell: optimization of process variables. Desalin Water Treat. 2013;51:1954–65. Funding Faraji M, Yamini Y, Shariati S. Application of cotton as a solid phase extraction There is no any funding of this study. sorbent for on-line preconcentration of copper in water samples prior to inductively coupled plasma optical emission spectrometry determination. J Availability of data and materials Hazard Mater. 2009;166:1383–8. The data and the contents of our manuscript will be available for the readers Hongbo X, WanpingZ,XiaoshunZ,Jing W,JianW.Simultaneouspreconcentrationof of the Journal of Analytical science and Technology. cobalt, nickel and copper in water samples by cloud point extraction method and their determination by flame atomic absorption spectrometry. Procedia Authors’ contributions Environ Sci. 2013;18:258. 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Journal
"Journal of Analytical Science and Technology" – Springer Journals
Published: Dec 1, 2018
Keywords: Analytical Chemistry; Characterization and Evaluation of Materials; Monitoring/Environmental Analysis