Dilek ESKİKÖY BAYRAKTEPE, Ceren YILDIZ, Zehra YAZAN

NiO Modifiye Karbon Pasta Sensör Yüzeyinde Bakır ve Kadmiyum‟un Anodik Sıyırma Voltametrisi ile Bir arada Tayini

Bu çalışmada NiO nanopartiküllerine dayanan, hızlı, duyarlı, düşük maliyetli yeni bir karbon pasta elektrotgeliştirilmesi ve bu elektrodun differansiyel puls anodik sıyırma voltametrisi (DPASV) yöntemiyle musluksuyunda bulunan Cu2+ ve Cd2+‟un analizinde kullanılması amaçlanmıştır. Bu amaç doğrultusunda, çıplak karbonpasta elektrot (KPE) ve NiO nanopartikülleriyle modifiye edilmiş olan karbon pasta elektrot (NiO/KPE)yüzeyleri EIS ve CV yöntemiyle yapılan karakterizasyon yöntemleri ile karşılaştırılmıştır. Elde edilen sonuçlar,NiO/KPE‟un elektroaktif türlere karşı elektrokatalitik etkisinin olduğunu göstermiş ve NiO/KPE, Cu2+ veCd2+‟un voltametrik analizinde çalışma elektrodu olarak kullanılmıştır. Çalışma elektrodunun belirlenmesininardından, bazı analitik ve yöntem parametrelerinin optimizasyonu yapılmış olup, her iki katyon için; optimumNiO bileşimi 3,0 mg NiO/30 mg pasta, optimum pH BR tampon ortamında 3,0, optimum biriktirme potansiyeli -1,5 V ve optimum biriktirme süresi ise 180,0 s olarak belirlenmiştir. Belirlenmiş olan optimum koşullarda, birkatyonun derişimi sabit tutulup, diğerinin derişimi arttırılarak ve her iki katyonun da derişimi arttırılarakkalibrasyon eğrileri oluşturulmuştur. Kalibrasyon eğrilerinden elde edilen veriler yardımıyla bulunan alt tayinsınırı ve doğrusal çalışma aralıkları her bir katyon için hesaplanmıştır. Yöntemin uygulanabilirliğinin testedilmesi amacıyla, musluk suyu içeren ortamda da Cu2+ ve Cd2+‟un analizi yeni geliştirilmiş olan DPASVyöntemiyle yapılmış ve geri kazanı değerleri %100 civarında bulunmuştur.

Anodic Stripping Voltammetric and Simultaneous Analysis of Cupper and Cadmium by Using NiO Nanoparticles Based Carbon Paste Sensor

In this study, we focused the development of a sensitive, fast and cost effective carbon paste electrode based on NiO (NiO/CPE) nanoparticles and a differential puls anodic adsorptive stripping voltammetric method (DPASV) for trace analysis of Cu2+ and Cd2+. For this purpose, the electrode surfaces of CPE and NiO/CPE were characterized by using EIS and CV methods. According to the results obtained, the NiO/CPE have electrocatalytic effect towards to the electroactive species compared to the bare CPE and in this study, this electrode was used as working electrode for simultaneous analysis of Cu2+ and Cd2+. The effect of pH, the composition of NiO, accumulation time and accumulation potential was optimized for reaching best response of Cu2+ and Cd2+ and optimum NiO content was selected as 3,0 mg NiO/30 mg paste, optimum pH in BR buffer solution 3,0, optimum deposition potential -1.5 V and optimum deposition time 180 s. The calibration graphs were created by using optimum conditions for Cu2+ and Cd2+both simultaneously and alone. The LOD and linear working ranges for each cation were calculated by using calibration studies. For testing applicability of newly developed method, Cu2+ and Cd2+ spiked in tap water and the analysis of these cations were carried out by using new DPASV method and the recovery results obtained were very satisfactorily.

PDF

___

[1] B. Sağlamtimur, B.Cicik ve C. Erdem “Kısa süreli bakır-kadmiyum etkileşiminde Tatlısu Çipurası (Oreochromis niloticus L. 1758)'nın karaciğer, böbrek, solungaç ve kas dokularındaki kadmiyum birikimi” Ekoloji, c. 14, s. 53, ss.33-38, 2004.
[2] Z. Koudelkova, T. Syrovy, P. Ambrozova, Z. Moravec, L. Kubac, D. Hynek ve V. Adam “Determination of zinc, cadmium, lead, copper and silver using a carbon paste electrode and a screen printed electrode modified with chromium (III) oxide” Sensors, vol. 17, no. 8, pp. 1832-1849, 2017.
[3] J.L. Gardea-Torresdey, J.R Peralta-Videa, M. Montes, G. De la Rosa ve B. “Corral-Diaz Bioaccumulation of cadmium, chromium and copper by Convolvulus arvensis L.: impact on plant growth and uptake of nutritional elements” Bioresource technology, vol. 9 no. 3, pp. 229-235, 2004.
[4] A. Cherfi, S. Abdoun ve O. Gaci “Food survey: levels and potential health risks of chromium, lead, zinc and copper content in fruits and vegetables consumed in Algeria” Food and chemical toxicology, vol. 70, pp. 48-53, 2014.
[5] G.J. Fosmire “Zinc toxicity” The American journal of clinical nutrition, vol. 51, no. 2 pp. 225-227, 1990.
[6] G. Özbolat ve A. Tuli, “Ağır metal toksisitesinin insan sağlığına etkileri” Arşiv Kaynak Tarama Dergisi, c. 25, s. 4, ss. 502-521, 2016.
[7] U. Injang, P. Noyrod, W. Siangproh, W. Dungchai, S. Motomizu ve O. Chailapakul “Determination of trace heavy metals in herbs by sequential injection analysis-anodic stripping voltammetry using screen-printed carbon nanotubes electrodes” Analytica chimica acta, vol. 668, no. 1, pp. 54-60, 2010.
[8] M.M. Ghoneim, A.M. Hassanein, E. Hammam ve A.M. Beltagi “Simultaneous determination of Cd, Pb, Cu, Sb, Bi, Se, Zn, Mn, Ni, Co and Fe in water samples by differential pulse stripping voltammetry at a hanging mercury drop electrode” Fresenius' journal of analytical chemistry, vol. 367 no. 4, pp. 378-383, 2000.
[9] S. Daniele, M.A. Baldo, P. Ugo ve G.A. Mazzocchin “Determination of heavy metals in real samples by anodic stripping voltammetry with mercury microelectrodes: Part 1. Application to wine” Analytica Chimica Acta, vol. 219, pp. 9-18, 1989.
[10] J. Golimowski ve A. Sikorska “A Voltammetric Method of the Determination of Toxic Heavy-Metals In Surface Waters” Chemia Analityczna, vol. 28, no. 4, pp. 411-420, 1983.
[11] E. Tesarova, L. Baldrianova, S. Hocevar, I. B. Svancara, K. Vytras ve B. Ogorevc “Anodic stripping voltammetric measurement of trace heavy metals at antimony film carbon paste electrode” Electrochimica Acta, vol. 54, no. 5, pp. 1506-1510, 2009.
[12] C. Hu, Wu, K., Dai, X., & Hu, S. (2003). Simultaneous determination of lead (II) and cadmium (II) at a diacetyldioxime modified carbon paste electrode by differential pulse stripping voltammetry. Talanta, vol. 60, no. 1, pp. 17-24.
[13] W. Yantasee, Y. Lin, G.E. Fryxell ve B.J. Busche “Simultaneous detection of cadmium, copper, and lead using a carbon paste electrode modified with carbamoylphosphonic acid self-assembled monolayer on mesoporous silica (SAMMS)” Analytica Chimica Acta, vol. 502, no. 2, pp. 207-212, 2004.
[14] M. Zaib ve M.M. Athar “Voltammetric Detection of Hg (II) in Real Wastewater Using Red Alga Modified Carbon Paste Electrode: Mechanism Insight” Arabian Journal for Science and Engineering, vol. 44 no. 1, pp. 179-187, 2019.
[15] D.E. Bayraktepe, T. Yanardağ, Z. Yazan ve A. Aksüt “Voltammetric determination of etoposide by using sepiolite clay modified electrode and its interaction with DNA” Rev. Roum. Chim, vol. 60, no. 4, pp. 287-295, 2015.
[16] S. Aydar, D.E. Bayraktepe, H. Filik ve Z. Yazan “A Nano˗ Sepiolite Clay Electrochemical Sensor for the Rapid Electro–Catalytic Detection of Hydroquinone in Cosmetic Products” Acta Chimica Slovenica, vol. 65 no. 4, pp. 946-954, 2018.
[17] H. Khani, M.K. Rofouei, P. Arab, V.K. Gupta ve Z. Vafaei “Multi-walled carbon nanotubesionic liquid-carbon paste electrode as a super selectivity sensor: application to potentiometric monitoring of mercury ion (II)” Journal of hazardous materials, vol. 183, no.1-3, pp. 402- 409, 2010.
[18] S.M. Ghoreishi, M. Behpour ve M. Golestaneh “Simultaneous determination of sunset yellow and tartrazine in soft drinks using gold nanoparticles carbon paste electrode” Food chemistry, vol. 132, no.1, pp. 637-641, 2012.
[19] M. Mazloum-Ardakani, H. Beitollahi, M.K. Amini, F. Mirkhalaf ve M. Abdollahi-Alibeik “New strategy for simultaneous and selective voltammetric determination of norepinephrine, acetaminophen and folic acid using ZrO2 nanoparticles-modified carbon paste electrode” Sensors and Actuators B: Chemical, vol.151 no. 1, pp. 243-249, 2010.
[20] J. Wang ve A. Walcarius “Zeolite-modified carbon paste electrode for selective monitoring of dopamine” Journal of Electroanalytical Chemistry, vol. 407, no.1-2, pp. 183-187, 1996.
[21] H. R. Zare, N. Nasirizadeh ve M.M. Ardakani “Electrochemical properties of a tetrabromop-benzoquinone modified carbon paste electrode. Application to the simultaneous determination of ascorbic acid, dopamine and uric acid” Journal of Electroanalytical Chemistry, vol. 577 no.1, pp. 25-33, 2005.
[22] F. Li, J. Li, Y. Feng, L. Yang ve Z. Du “Electrochemical behavior of graphene doped carbon paste electrode and its application for sensitive determination of ascorbic acid” Sensors and actuators B: Chemical vol.157, no.1, pp. 110-114, 2011.
[23] A. Salimi, E. Sharifi, A. Noorbakhsh and S. Soltanian “Direct voltammetry and electrocatalytic properties of hemoglobin immobilized on a glassy carbon electrode modified with nickel oxide nanoparticles” Electrochemistry communications, vol. 8, no.9, pp. 1499-1508, 2006.
[24] M.R Shahmiri, A. Bahari, H. Karimi-Maleh, R. Hosseinzadeh and N. Mirnia “Ethynylferrocene–NiO/MWCNT nanocomposite modified carbon paste electrode as a novel voltammetric sensor for simultaneous determination of glutathione and acetaminophen” Sensors and Actuators B: Chemical, vol.177, pp.70-77, 2013.
[25] H. Karimi-Maleh, A.L. Sanati, V.K. Gupta, M. Yoosefian, M. Asif and A. Bahari, “A voltammetric biosensor based on ionic liquid/NiO nanoparticle modified carbon paste electrode for the determination of nicotinamide adenine dinucleotide (NADH)” Sensors and Actuators B: Chemical, vol.204, pp.647-654, 2014.
[26] S. Jahani ve H. Beitollahi “Selective detection of dopamine in the presence of uric acid using NiO nanoparticles decorated on graphene nanosheets modified screen‐ printed electrodes” Electroanalysis, vol. 28, no. 9, pp. 2022-2028, 2016.
[27] D.E. Bayraktepe, Z. Yazan ve K. Polat “Sensitive and selective voltammetric determination of anti˗ cancer agent shikonin on sepiolite clay/TiO2 nanoparticle/MWCNTs composite carbon paste sensor and investigation of its electro˗ oxidation mechanism” Journal of Electroanalytical Chemistry, vol. 780, pp. 38-45, 2016.
[28] J. Wang, Analytical electrochemistry, John Wiley & Sons, 2006.
[29] A.M. Beltagi, E.M. Ghoneim ve M.M. Ghoneim “Simultaneous determination of cadmium (II), lead (II), copper (II) and mercury (II) by square wave anodic stripping voltammetry at a montmorillonite-calcium modified carbon paste electrode” International Journal of Environmental and Analytical Chemistry, vol. 91, no. 1, pp. 17-32, 2011.
[30] H. Lin, M. Li, D. Mihailovič “Simultaneous Determination of Copper, Lead, and Cadmium Ions at a Mo6S9-xIx Nanowires Modified Glassy Carbon Electrode Using Differential Pulse Anodic Stripping Voltammetry” Electrochimica Acta, vol. 154, pp. 184–189, 2015.
[31] N. Serrano, A. González-Calabuig M. Valle “Crownether-modified electrodes for the simultaneous stripping voltammetric determination of Cd(II), Pb(II) and Cu(II)”, Talanta vol.138, pp. 130–137, 2015.
[32] Z. Guo, D. Li, X. Luo “Simultaneous determination of trace Cd(II), Pb(II) and Cu(II) by differential pulse anodic stripping voltammetry using a reduced graphene oxide chitosan/poly-L-lysine nanocomposite modified glassy carbon electrode” Journal of Colloid and Interface Science vol. 490, pp. 11–22, 2017.
[33] X. Han, Z. Meng, H. Zhang ve J. Zheng “Fullerene-based anodic stripping voltammetry for simultaneous determination of Hg(II), Cu(II), Pb(II) and Cd(II) in foodstuff” Microchimica Acta (2018) vol. 185, no. 274, pp. 1-9.