In this research, an eco-friendly magnetic adsorbent based on Fe3O4/salicylic acid nanocomposite was fabricated using a facile one-pot co-precipitation method. The crystalline and morphological characterization of the prepared nanocomposite was performed by field emission scanning electron microscopy, X-ray diffraction, and Fourier transform infrared spectroscopy. The nanocomposite was employed as a magnetic solid-phase extraction agent for separation of Cd(II) ions from synthetic solutions. Some experimental factors affecting the extraction efficiency were investigated and optimized. Following elution with acetic acid (pH 3.5), the pre-concentrated analyte was quantified by flame atomic absorption spectrometry. In optimal conditions, a linear calibration graph was achieved in the concentration range of 0.2–30 ng·mL−1 with a determination coefficient (R2) of 0.9953. The detection limit, the enhancement factor, inter- and intra-day relative standard deviations (for six consecutive extractions at the concentration level of 10 ng·mL−1) were 0.04 ng·mL−1, 100, 2.38% and 1.52%, respectively. To evaluate the accuracy of the method, a certified reference material (NIST SRM 1643e) was analyzed, and there was a good agreement between the certified and the measured values. It was successfully utilized to determine cadmium in industrial wastewater samples and the attained relative recovery values were between 96.8% and 103.2%.
. [J]. Frontiers of Chemical Science and Engineering, 2021, 15(2): 450-459.
Hossein Abdolmohammad-Zadeh, Arezu Salimi. A magnetic adsorbent based on salicylic acid-immobilized magnetite nano-particles for pre-concentration of Cd(II) ions. Front. Chem. Sci. Eng., 2021, 15(2): 450-459.
M E Mahmoud, A A Yakout, K H Hussein, M M Osman. Magnetic accumulation and extraction of Cd(II), Hg(II) and Pb(II) by a novel nano-Fe3O4-coated-dioctylphthalate-immobilized-hydroxylamine. Journal of Environmental Chemical Engineering, 2015, 3(2): 843–851 https://doi.org/10.1016/j.jece.2015.03.024
2
G Xiang, Y Huang, Y Luo. Solid phase extraction of trace cadmium and lead in food samples using modified peanut shell prior to determination by flame atomic absorption spectrometry. Mikrochimica Acta, 2009, 165(1-2): 237–242 https://doi.org/10.1007/s00604-008-0126-y
3
M H Mashhadizadeh, Z Karami. Solid phase extraction of trace amounts of Ag, Cd, Cu, and Zn in environmental samples using magnetic nanoparticles coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1, 3, 4-thiadiazole and their determination by ICP-OES. Journal of Hazardous Materials, 2011, 190(1-3): 1023–1029 https://doi.org/10.1016/j.jhazmat.2011.04.051
4
M Tuzen, S Sahiner, B Hazer. Solid phase extraction of lead, cadmium and zinc on biodegradable polyhydroxybutyrate diethanol amine (PHB-DEA) polymer and their determination in water and food samples. Food Chemistry, 2016, 210: 115–120 https://doi.org/10.1016/j.foodchem.2016.04.079
5
A Mirabi, Z Dalirandeh, A Shokuhi Rad. Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry. Journal of Magnetism and Magnetic Materials, 2015, 381: 138–144 https://doi.org/10.1016/j.jmmm.2014.12.071
6
H Ciftci. Separation and solid phase extraction method for the determination of cadmium in environmental samples. Desalination, 2010, 263(1-3): 18–22 https://doi.org/10.1016/j.desal.2010.06.028
7
Y Zhai, Y Liu, X Chang, S Chen, X Huang. Selective solid-phase extraction of trace cadmium (II) with an ionic imprinted polymer prepared from a dual-ligand monomer. Analytica Chimica Acta, 2007, 593(1): 123–128 https://doi.org/10.1016/j.aca.2007.04.040
8
A Banazadeh, S Mozaffari, B Osoli. Facile synthesis of cysteine functionalized magnetic graphene oxide nanosheets: application in solid phase extraction of cadmium from environmental sample. Journal of Environmental Chemical Engineering, 2015, 3(4): 2801–2808 https://doi.org/10.1016/j.jece.2015.10.003
9
T Dong, L Yang, M Zhu, Z Liu, X Sun, J Yu, H Liu. Removal of cadmium (II) from wastewater with gas-assisted magnetic separation. Chemical Engineering Journal, 2015, 280: 426–432 https://doi.org/10.1016/j.cej.2015.05.066
10
T Daşbaşı, S Saçmacı, A Ülgen, S Kartal. A solid phase extraction procedure for the determination of Cd (II) and Pb (II) ions in food and water samples by flame atomic absorption spectrometry. Food Chemistry, 2015, 174: 591–596 https://doi.org/10.1016/j.foodchem.2014.11.049
11
S A Rezvani, A Soleymanpour. Application of L-cystine modified zeolite for preconcentration and determination of ultra-trace levels of cadmium by flame atomic absorption spectrometry. Journal of Chromatography. A, 2016, 1436: 34–41 https://doi.org/10.1016/j.chroma.2016.01.065
12
Y Zhu, K Chiba. Determination of cadmium in food samples by ID-ICP-MS with solid phase extraction for eliminating spectral-interferences. Talanta, 2012, 90: 57–62 https://doi.org/10.1016/j.talanta.2011.12.071
13
Y Suzuki, Y Endo, M Ogawa, M Matauda, Y Nakajima, N Onda, M Iwasaki, S Tsugane. A Determination of sub-ppb cadmium in urine by solid-phase extraction and inductively coupled plasma-mass spectrometry. Analytical Sciences, 2008, 24(8): 1049–1052 https://doi.org/10.2116/analsci.24.1049
14
M Krawczyk, M Jeszka-Skowro. Multiwalled carbon nanotubes as solid sorbent in dispersive micro solid-phase extraction for the sequential determination of cadmium and lead in water samples. Microchemical Journal, 2016, 126: 296–301 https://doi.org/10.1016/j.microc.2015.12.027
15
S Z Mohammadi, D Afzali, D Pourtalebi. Flame atomic absorption spectrometric determination of trace amounts of lead, cadmium and nickel in different matrixes after solid phase extraction on modified multiwalled carbon nanotubes. Open Chemistry, 2010, 8(3): 662–668 https://doi.org/10.2478/s11532-010-0029-8
16
K Prasad, P Gopikrishna, R Kala, T Prasada Rao, G R K Naidu. Solid phase extraction vis-a-vis coprecipitation preconcentration of cadmium and lead from soils onto 5, 7-dibromoquinoline-8-ol embedded benzophenone and determination by FAAS. Talanta, 2006, 69(4): 938–945 https://doi.org/10.1016/j.talanta.2005.11.040
17
X Huang, X Chang, Q He, Y Cui, Y Zhai, N Jiang. Tris(2-aminoethyl) amine functionalized silica gel for solid-phase extraction and preconcentration of Cr (III), Cd (II) and Pb (II) from waters. Journal of Hazardous Materials, 2008, 157(1): 154–160 https://doi.org/10.1016/j.jhazmat.2007.12.113
18
M Behbahani, A Bagheri, M M Amini, O Sadeghi, M Salarian, F Najafi, M Taghizadeh. Application of multiwalled carbon nanotubes modified by diphenylcarbazide for selective solid phase extraction of ultra-traces Cd(II) in water samples and food products. Food Chemistry, 2013, 141(1): 48–53 https://doi.org/10.1016/j.foodchem.2013.03.011
19
C Duran, A Gundogdu, V N Bulut, M Soylak, L Elci, H B Senturk, M Tufekci. Solid-phase extraction of Mn (II), Co (II), Ni (II), Cu (II), Cd (II) and Pb (II) ions from environmental samples by flame atomic absorption spectrometry (FAAS). Journal of Hazardous Materials, 2007, 146(1-2): 347–355 https://doi.org/10.1016/j.jhazmat.2006.12.029
20
M Tuzen, K O Saygi, M Soylak. Solid phase extraction of heavy metal ions in environmental samples on multiwalled carbon nanotubes. Journal of Hazardous Materials, 2008, 152(2): 632–639 https://doi.org/10.1016/j.jhazmat.2007.07.026
21
Z A Alothman, M Habila, E Yilmaz, M Soylak. Solid phase extraction of Cd (II), Pb (II), Zn (II) and Ni (II) from food samples using multiwalled carbon nanotubes impregnated with 4-(2-thiazolylazo) resorcinol. Mikrochimica Acta, 2012, 177(3-4): 397–403 https://doi.org/10.1007/s00604-012-0789-2
22
M Tuzen, K Parlar, M Soylak. Enrichment/separation of cadmium (II) and lead (II) in environmental samples by solid phase extraction. Journal of Hazardous Materials, 2005, 121(1-3): 79–87 https://doi.org/10.1016/j.jhazmat.2005.01.015
23
I S Barreto, S I E Andrade, F A S Cunha, M B Lima, M Araujo, L F Almeida. A robotic magnetic nanoparticle solid phase extraction system coupled to flow-batch analyzer and GFAAS for determination of trace cadmium in edible oils without external pretreatment. Talanta, 2018, 178: 384–391 https://doi.org/10.1016/j.talanta.2017.09.063
24
N Zhang, H Peng, S Wang, B Hu. Fast and selective magnetic solid phase extraction of trace Cd, Mn and Pb in environmental and biological samples and their determination by ICP-MS. Mikrochimica Acta, 2011, 175(1-2): 121–128 https://doi.org/10.1007/s00604-011-0659-3
25
B Cai, J Yin, Y H Hao, Y N Li, B F Yuan, Y Q Feng. Profiling of phytohormones in rice under elevated cadmium concentration levels by magnetic solid-phase extraction coupled with liquid chromatography tandem mass spectrometry. Journal of Chromatography. A, 2015, 1406: 78–86 https://doi.org/10.1016/j.chroma.2015.06.046
26
W Gu, X Zhu. Nanoparticles of type Fe3O4-SiO2-graphene oxide and coated with an amino acid-derived ionic liquid for extraction of Al (III), Cr (III), Cu (II), Pb (II) prior to their determination by ICP-OES. Mikrochimica Acta, 2017, 184(11): 4279–4286 https://doi.org/10.1007/s00604-017-2469-8
27
Y Jia, Y Wang, M Yan, Q Wang, H Xu, X Wang, H Zhou, Y Hao, M Wang. Fabrication of iron oxide@ MOF-808 as a sorbent for magnetic solid phase extraction of benzoylurea insecticides in tea beverages and juice samples. Journal of Chromatography. A, 2020, 1615:460766
28
R A Andrade, F A Cunha, S I Andrade, P L Junior, L A Navarro, W S Lyra, A G Pessoa, R A Lima, M C U Araujo. A digital capture movie-based robotized Flow-batch luminometer for in-line magnetic nanoparticle solid phase extraction and chemiluminescent measurement. Microchemical Journal, 2020, 153: 104387 https://doi.org/10.1016/j.microc.2019.104387
29
Y Zhao, R Wu, H Yu, J Li, L Liu, S Wang, X Chen, T W D Chan. Magnetic solid-phase extraction of sulfonamide antibiotics in water and animal-derived food samples using core-shell magnetite and molybdenum disulfide nanocomposite adsorbent. Journal of Chromatography. A, 2020, 1610: 460543 https://doi.org/10.1016/j.chroma.2019.460543
30
M E Mahmoud, A A Soayed, O F Hafez. Selective solid phase extraction and pre-concentration of heavy metals from seawater by physically and chemically immobilized 4-amino-3-hydroxy-2-(2-chlorobenzene)-azo-1-naphthalene sulfonic acid silica gel. Mikrochimica Acta, 2003, 143(1): 65–70 https://doi.org/10.1007/s00604-003-0046-9
31
I Mindrila, S A Buteica, D E Mihaiescu, G Badea, A Fudulu, D N Margaritescu. Fe3O4/salicylic acid nanoparticles versatility in magnetic mediated vascular nanoblockage. Journal of Nanoparticle Research, 2016, 18(1): 10–20 https://doi.org/10.1007/s11051-015-3318-5
32
D E Mihaiescu, A S Buteica, J Neamtu, D Istrati, I Mindrila. Fe3O4/salicylic acid nanoparticles behavior on chick CAM vasculature. Journal of Nanoparticle Research, 2013, 15(8): 1857–1867 https://doi.org/10.1007/s11051-013-1857-1
33
B Unal, Z Durmus, H Kavas, A Baykal, M S Toprak. Synthesis, conductivity and dielectric characterization of salicylic acid-Fe3O4 nanocomposite. Materials Chemistry and Physics, 2010, 123(1): 184–190 https://doi.org/10.1016/j.matchemphys.2010.03.080
34
Y Cui, X Chang, X Zhu, X Zou. Selective solid phase extraction of trace cadmium(II) and lead(II) from biological and natural water samples by ofloxacin-modified-silica gel. International Journal of Environmental Analytical Chemistry, 2008, 88(12): 857–868 https://doi.org/10.1080/03067310802208360
35
F An, B Gao, X Dai, M Wang, X Wang. Efficient removal of heavy metal ions from aqueous solution using salicylic acid type chelate adsorbent. Journal of Hazardous Materials, 2011, 192(3): 956–962 https://doi.org/10.1016/j.jhazmat.2011.05.050
36
J H Ephraim, H Xu. The binding of cadmium by an aquatic fulvic acid: A comparison of ultrafiltration with ion‒exchange distribution and ion-selective electrode techniques. Science of the Total Environment, 1989, 81: 625–634 https://doi.org/10.1016/0048-9697(89)90171-X
37
H Abdolmohammad-Zadeh, E Rahimpour, A Hosseinzadeh, M Zamani-Kalajahi. Aluminum(III)-doped ZnO@Fe3O4 nanocomposite as a magnetic sorbent for preconcentration of cadmium (II). Mikrochimica Acta, 2017, 184(6): 1641–1648 https://doi.org/10.1007/s00604-017-2166-7
38
A Afkhami, T Madrakian, R Ahmadi, H Bagheri, M Tabatabaee. Chemically modified alumina nanoparticles for selective solid phase extraction and preconcentration of trace amounts of Cd (II). Mikrochimica Acta, 2011, 175(1-2): 69–77 https://doi.org/10.1007/s00604-011-0660-x
39
E B Kafa, M Firat, D S Chormey, F Turak, S Bakırdere. Sensitive determination of cadmium in lake water, municipal wastewater and onion samples by slotted quartz tube-flame atomic absorption spectrometry after preconcentration with microextraction strategy. Measurement, 2018, 125: 219–223 https://doi.org/10.1016/j.measurement.2018.04.068
40
B Zargar, A Khazaeifar. Synthesis of an ion-imprinted sorbent by surface imprinting of magnetized carbon nanotubes for determination of trace amounts of cadmium ions. Mikrochimica Acta, 2017, 184(11): 4521–4529 https://doi.org/10.1007/s00604-017-2489-4
41
J M Sousa, M T Couto, R J Cassell. Polyurethane foam functionalized with phenylfluorone for online preconcentration and determination of copper and cadmium in water samples by flame atomic absorption spectrometry. Microchemical Journal, 2018, 138: 92–97 https://doi.org/10.1016/j.microc.2018.01.006
42
E O Er, E Maltepe, S Bakirdere. A novel analytical method for the determination of cadmium in sorrel and rocket plants at ultratrace levels: Magnetic chitosan hydrogels based solid phase microextraction-slotted quartz tube-flame atomic absorption spectrophotometry. Microchemical Journal, 2018, 143: 393–399 https://doi.org/10.1016/j.microc.2018.08.019
43
Z Dahaghin, H Zavvar Mousavi, E Mirparizi, P Haghighat. Synthesis and application of a novel magnetic nanosorbent for determination of trace Cd (II), Ni (II), Pb (II), and Zn (II) in environmental samples. Chemical Papers, 2018, 72(6): 1451–1459 https://doi.org/10.1007/s11696-018-0387-9
44
M H Kojidi, A Aliakbar. A graphene oxide based poly (2,6-diaminopyridine) composite for solid-phase extraction of Cd (II) prior to its determination by FAAS. Mikrochimica Acta, 2017, 184(8): 2855–2860 https://doi.org/10.1007/s00604-017-2317-x
45
Z Dahaghin, H Zavvar Mousavi, M Sajjadi. Trace amounts of Cd (II), Cu (II) and Pb (II) ions monitoring using Fe3O4@ graphene oxide nanocomposite modified via 2-mercaptobenzothiazole as a novel and efficient nanosorbent. Journal of Molecular Liquids, 2017, 231: 386–395 https://doi.org/10.1016/j.molliq.2017.02.023
46
E Ghorbani-Kalhor. A metal-organic framework nanocomposite made from functionalized magnetite nanoparticles and HKUST-1 (MOF-199) for preconcentration of Cd (II), Pb (II), and Ni (II). Mikrochimica Acta, 2016, 183(9): 2639–2647 https://doi.org/10.1007/s00604-016-1896-2
47
M A Farajzadeh, A Yadeghari. Extraction and preconcentration of nickel, cadmium, cobalt, and lead cations using dispersive solid phase extraction performed in a narrow-bore tube. Journal of Industrial and Engineering Chemistry, 2018, 59: 377–387 https://doi.org/10.1016/j.jiec.2017.10.046
48
Q Zhou, M Lei, Y Liu, Y Wu, Y Yuan. Simultaneous determination of cadmium, lead and mercury ions at trace level by magnetic solid phase extraction with Fe@Ag@Dimercaptobenzene coupled to high performance liquid chromatography. Talanta, 2017, 175: 194–199 https://doi.org/10.1016/j.talanta.2017.07.043
49
Y Yuan, Y Wu, H Wang, Y Tong, X Sheng, Y Sun, X Zhou, Q Zhou. Simultaneous enrichment and determination of cadmium and mercury ions using magnetic PAMAM dendrimers as the adsorbents for magnetic solid phase extraction coupled with high performance liquid chromatography. Journal of Hazardous Materials, 2020, 386: 121658 https://doi.org/10.1016/j.jhazmat.2019.121658