Preconcentration of Iron in Some Drug and Water Samples by Coprecipitation with Magnesium Hydroxide Before Spectrophotometric Determination

Yıl 2018, Cilt: 39 Sayı: 1, 218 - 232, 16.03.2018

Cemalettin Uyan Ersin Bekçioğulları

https://doi.org/10.17776/csj.353455

Öz

A method was purposed for preconcentration and determination of iron, in this
study. The method consist of these steps respectively: I) Coprecipitation of
the iron present in the sample with Mg(OH)₂ collector. II)
Seperation of the precipitate by centrifuging. III) Solving the precipitation
in acid. IV) UV-VIS spectrophotometric determination of the iron concentrated
in the resultant lower volume solution using its complexation with thiocyanate.
The effects of factors such as centrifugation time, pH and Mg concentration on
the absorbance signal were investigated and the optimum values of these factors
were determined. Total iron in the sample was brought single oxidation state
(Fe(II) or Fe(III)) before coprecipitation procedure. Calibration
curve was derived for both of the proceses. The detection limit and working
range for the proposed method were found to be 0.01 mgL^-1 and
0.03-0.3 mgL^-1 respectively. The proposed method was applied to tap
water, mineral water samples and Rennie anti-acid drug tablet. The accuracy of
the method was tested by analyte spiked method. The accuracy results in terms
of Recovery % are between 90-100%. Mostly the relative standart deviations (RSD
%) values do not exceed 5%. 

Anahtar Kelimeler

preconcentration, coprecipitation, Mg(OH)2 collector, Iron determination, UV-VIS absorpsiyon spectrophotometric method

Bazı ilaç ve Su Örneklerinde Demirin Spektrofotometrik Tayin Öncesi Mağnezyum Hidroksit ile Birlikte Çöktürme Yoluyla Önderiştirilmesi

Öz

Bu çalışmada demir için bir önderiştirme ve
tayin yöntemi önerilmektedir. Yöntem
sırasıyla şu adımlardan ibarettir: I) Mg(OH)₂ kollektörüyle
örnekteki demirin birlikte çökmesi II) Oluşan çökeleğin santrifüjlenerek
ayrılması, III) Çökeleğin asitte çözülmesi IV) Elde edilen daha düşük hacimli
çözeltide deriştirilmiş olan demirin tiyosiyanatla kompleksleşme yoluyla UV-VIS
spektrofotometrik olarak tayin edilmesi. Santrifüjleme süresi, pH, Mg derişimi
gibi etkenlerin çökmeye veya absorbans sinyaline etkileri araştırılmış ve bu
etkenlerin optimum değerleri belirlenmiştir. Örnekteki toplam demir, birlikteçöktürme öncesi tek bir
yükseltgenme haline (Fe(II) or Fe(III) ) dönüştürmüştür. Prosesin her ikisi
için kalibrasyon grafiği oluşturulmuştur.  Yönteme ait 0,01mgL^-1 tespit sınırı
ve 0,03-0,3 mgL^-1 çalışma aralığı elde edilmiştir. Yöntem musluk
suyuna, maden suyu örneklerine ve Rennie antiasit ilaç tabletine
uygulanmıştır.  Yöntemin doğruluğu analit
aşılama yoluyla test edilmiştir. Elde edilen doğruluk değerlerinin çoğu yüzde
geri kazanım olarak % 90-100 arasındadır. 
Tekrarlanabilirlik veya kesinlik için ise bağıl standart sapma olarak
çoğunluğu % 5’i geçmeyen değerler elde edilmiştir.  

Anahtar Kelimeler

Demir tayini, demir önderiştirilmesi, birlikte çöktürme, Mg(OH)2 kollektörü, UV-VIS Spektrofotometrik metod

Kaynakça

• [1]. Minczewski J., Chwastowska J., Dybczynski J., Seperation and Preconcentration Methods in Inorganic Trace Analysis, Ellis Horwood Chichester. (1982) 39-56,
• [2]. Okochi H., Sudo E. Separation of micro quantities of bismuth and iron in lead by EDTA masking-coprecipitation method, Bunseki Kagaku, 22-4 (1973) 431-437 NKI.
• [3]. K Kitson, R.E., Smultaneous Spectrophotometric Determination of Cobalt, Copper and Iron, Analytical Chemistry,22-5 ( 1950) 664.
• [4]. Bode, H., On Sandell’s sensivity, Fresenius J Anal Chem., 339 (1991) 898.
• [5]. Elçi L., Şahin U., Öztaş S., Determination of trace amounts of some metals in samples with high salt content by atomic absorption spectrometry after cobalt-diethyldithiocarbamate coprecipitation, Talanta 44 (1997) 1017-1023.
• [6]. Wu J., Boyle E. A., Determination of iron in seawater by high-resolution isotope dilution inductively coupled plasma mass spectrometry after Mg(OH)2 coprecipitation, Analytica Chimica Acta, 367 (1998) 183-191.
• [7]. Ata Atanassova D., Stefanova V., Russeva E., , Co-precipitative preconcentration with sodium diethyldithiocarbamate and ICP-AES determination of Se, Cu, Pb, Zn, Fe, Co, Ni, Mn, Cr and Cd in water. Talanta, 47 (1998) 1237–1243.
• [8]. Kagaya S., M. Saiki · Z. A. Malek, Y. Araki ·K. Hasegawa, Coprecipitation with lanthanium phosphate as a technique for separation and preconcentration of iron(III) and lead. Fresenius J Anal. Chem., 371 (2001) 391–393.
• [9]. Umashankar V., Radhamani R., Ramadoss K., Murty. D.S.R., Simultaneous separation and preconcentration of trace elements in water samples by coprecipitation on manganese dioxide using D-glucose as reductant for KMnO4, Talanta, 57 (2002) 1029-1038.
• [10]. Elçi L., Soylak M. And Özcan B., Coprecipitation of Cu(II), Ni(II), Fe(III), Cd(II), Pb(II) and Co(II) in Wastewater, Sediment, and Metallic Zinc Samples with HMDTC–HMA for Flame Atomic Absorption Spectrometric Determination, Analytical Letter, 36-5 (2003) 987– 999.
• [11]. Soylak M., Saracoglu S., Divrikli Ü., Elçi L., Coprecipitation of heavy metals with erbium hydroxide for their flame atomic absorption spectrometric determinations in environmental samples, Talanta, 66 (2005) 1098–1102.
• [12]. Kagaya S., Araki Y., Hirai N., Hasegawa K., Coprecipitation with yitrium phosphate as a separation technique for iron(III), lead, and bismuth from cobalt, nickel, and copper matrices, Talanta, 67 (2005) 90–97
• [13]. Soylak M., Erdoğan N.D., Copper(II)–rubeanic acid coprecipitation system for separation–preconcentration of trace metal ions in environmental samples for their flame atomic absorption spectrometric determinations, Journal of Hazardous Materials B., 137 (2006) 1035–1041.
• [14]. Soylak M., Onal G., Determination of trace metals by atomic absorption spectrometry after coprecipitation with europium hydroxide, Journal of Hazardous Materials B, 137 (2005) 1130–1134.
• [15]. Saracoğlu Sibel, M. Soylak M., Peker D.S., L. Elci L., Santos W.N.L., Lemose V.A., Ferreira S..L.C., A preconcentration procedure using coprecipitation for determination of lead and iron in several samples using flame atomic absorption spectrometry, Analytica Chimica Acta, 575 (2006) 133–137.
• [16]. Saito M. A. And Schneider D. L., Examination of precipitation and improvements in precision using Mg(OH)2 preconcentration inductively coupled plasma mass spectrometry (ICP-MS) method for high-throughput analysis of open-ocean Fe and Mn in seaawater,Analytica Chimica Acta, 565 (2006) 222-233.
• [17]. Aydın A. F. ve Soylak M., A novel multi-element coprecipitation technique for separation and enrichment of metal ions in environmental samples. Talanta, 73 (2007) 134-141.
• [18]. Duran C., Bulut V. N., Gundogdu A., Ozdes D., Yildirim N., Soylak M., Senturk H. B., Elci L., Carrier element-free coprecipitation with 3-phenly-4-o-hydroxybenzylidenamino-4,5-dihydro-1,2,4-triazole-5-one (POHBAT) for separation/preconcentration of Cr(III), Fe(III), Pb(II) and Zn(II) from aqueous solutions, Journal of Hazardous Materials, 167- 1,3 (2009) 294-299.
• [19]. Kagaya Shigehiro, Mizuno Toshiyuki, Tohda Koji, Inductively Coupled plasma atomic emission spectrometric determination of 27 trace elements in table salts after coprecipitation with indium phosphate, Talanta, 79 (2009) 512–516.
• [20]. Tokalıoğlu S. & Yıldız S., A comparative study on the preconcentration of some metal ions in water samples with Cu(II) and Ni(II) salicylaldoxime coprecipitants, Microchim Acta, 165 (2009) 129–133. [21]. Citak Demirhan, Tuzen Mustafa, Soylak Mustafa, Simultaneous coprecipitation of lead, cobalt, copper, cadmium, iron and nickel in food samples with zirconium(IV) hydroxide prior to their flame atomic absorption spectrometric determination, Food and Chemical Toxicology, 47 (2009) 2302–2307.
• [22]. Grotti M., Francesco Soggia S. F., Ardini F. and Frache, R., Determination of subna-nomolar levels of iron in sea-water using reaction cell inductively coupled plasma mass spectrometry after Mg(OH)2 coprecipitation J. Anal. At. Spectrom., 24 (2009) 522-527.
• [23]. Saracoglu S., Soylak M., Carrier element-free coprecipitation (CEFC) method collector CTAB for separation and pre-concentration of some metal ions in natural water and soil samples, Food and Chemical Toxicology, 48 (2010) 1328–1333. [24]. Uluozlü D. Ö.,, Tuzen M., Mendil D., Soylak M., Coprecipitation of trace elements with Ni(II)-2-Nitroso-1-naphthol-4-sulfonic acid and their determination by flame atomic absorption spectrometry, Journal of Hazardous Materials, 176 (2010) 1032–1037
• [25]. Sacmacı S. ve Kartal S., Determination of some trace metal ions in Various samples by FAAS after separation/preconcentration by copper(II)- BPHA coprecipitation method, Original paper, Microchim Acta , 170 (2010) 75–82.
• [26]. Soylak M., Aydin A., Determination of some heavy metals food and environmental samples by flame atomic absorption spectrometry after coprecipitation, Food and Chemical Toxicology, 49-6 (2011) 1242-1248
• [27]. Tokalıoglu S., Ayhanoz H., Use of Cu(II) and Fe(III) N-benzoyl-N-phenylhydroxylamine coprecipitants for preconcentration of some trace metal ions in food samples, Food Chemistry,127 (2011) 359–363 .
• [28]. Mendil D., Karatas M., Tuzen M., Separation and preconcentration of Cu(II), Pb(II), Zn(II), Fe(III) and Cr(III) ions with coprecipitation method without carrier element and their determination in food and water samples. Food Chem., 177 (2015) 320-324.