Silica gel functionalized with resacetophenone: synthesis of a new chelating matrix and its application as metal ion collector for their flame atomic absorption spectrometric determination

被引:127
作者
Goswami, A [1 ]
Singh, AK [1 ]
机构
[1] Indian Inst Technol, Dept Chem, New Delhi 110016, India
关键词
resacetophenone; silica gel; preconcentration; chelating matrix; metal ions; atomic absorption spectrometry;
D O I
10.1016/S0003-2670(01)01552-5
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
Silica gel modified with 3-aminopropyltriethoxysilane was anchored with resacetophenone to prepare a new chelating surface (or matrix). It was characterized with cross polarization magic angle spinning C-13 NMR spectroscopy and diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy and used for the separation and preconcentration of Cu(II), Pb(II), Ni(II), Fe(III), Cd(II), Zn(II) and Co(II) prior to their determination by flame atomic absorption spectrometry (FAAS). The optimum pH ranges for quantitative sorption are 6.0-7.5, 5.5-7.5, 5.0-7.0, 6.5-7.5, 6.0-7.5, 6.0-7.0 and 6.0-7.5 for Cu, Pb, Fe, Zn, Co, Ni and Cd, respectively. All the metals can be desorbed with 3 mol dm(-3) HCI or HNO3. The sorption capacity for these metal ions is in range of 57.8-365.0 mumol g(-1) of chelating matrix. Tolerance limits for electrolytes NaNO3, NaCl, NaBr, Na2SO4 and Na3PO4 and cations Ca(II) and Mg(II) in the sorption of these metal ions are reported. Preconcentration factors of 200, 300, 150, 250, 250, 200 and 200 for Cd, Co, Zn, Cu, Pb, Fe and Ni, respectively, are obtained and t(1/2) values are < 1 min except for Cd. 95% extraction by a batch method takes < 25 min. The simultaneous enrichment and determination of all the metals are possible if the total load of the metal ions is less than the sorption capacity. In river water samples all these metal ions were enriched with the present matrix and determined with a flame atomic absorption spectrometer (R.S.D. < 7.7%). Copper contents of pharmaceutical samples (vitamin capsule) were preconcentrated with the present chelating matrix and estimated with flame AAS, with R.S.D. similar to 2.2%. The results are in the good agreement with the certified value, 0.4 mg/g of capsule. (C) 2002 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:229 / 240
页数:12
相关论文
共 39 条
[1]   Speciation of copper and manganese in milk by solid-phase extraction inductively coupled plasma-atomic emission spectrometry [J].
Abollino, O ;
Aceto, M ;
Bruzzoniti, MC ;
Mentasti, E ;
Sarzanini, C .
ANALYTICA CHIMICA ACTA, 1998, 375 (03) :299-306
[2]   SPECTROFLUOROMETRIC DETECTION-OF ZINC AND CADMIUM WITH 8-(BENZENESULFONAMIDO)-QUINOLINE IMMOBILIZED ON A POLYMERIC MATRIX [J].
COMPANO, R ;
FERRER, R ;
GUITERAS, J ;
PRAT, MD .
ANALYST, 1994, 119 (06) :1225-1228
[3]   Copper determination in natural water samples by using FAAS after preconcentration onto amberlite XAD-2 loaded with calmagite [J].
Ferreira, SLC ;
Ferreira, JR ;
Dantas, AF ;
Lemos, VA ;
Araújo, NML ;
Costa, ACS .
TALANTA, 2000, 50 (06) :1253-1259
[4]   Separation and preconcentration of cobalt after sorption onto amberlite XAD-2 loaded with 2-(2-thiazolylazo)-p-cresol [J].
Ferreira, SLC ;
de Brito, CF .
ANALYTICAL SCIENCES, 1999, 15 (02) :189-191
[5]   Nickel determination in saline matrices by ICP-AES after sorption on Amberlite XAD-2 loaded with PAN [J].
Ferreira, SLC ;
de Brito, CF ;
Dantas, AF ;
de Araújo, NML ;
Costa, ACS .
TALANTA, 1999, 48 (05) :1173-1177
[6]  
Gan NQ, 1998, ANALYST, V123, P2395
[7]   Solid-phase extraction of metal ions and their estimation in vitamins, steel and milk using 3-hydroxy-2-methyl-1,4-naphthoquinone-immobilized silica gel [J].
Garg, BS ;
Bist, JS ;
Sharma, RK ;
Bhojak, N .
TALANTA, 1996, 43 (12) :2093-2099
[8]   Separation and preconcentration of metal ions and their estimation in vitamin, steel and milk samples using o-vanillin-immobilized silica gel [J].
Garg, BS ;
Sharma, RK ;
Bist, JS ;
Bhojak, N ;
Mittal, S .
TALANTA, 1999, 48 (01) :49-55
[9]   PRECONCENTRATION OF TRACE-METALS FROM SEAWATER WITH 7-DODECENYL-8-QUINOLINOL IMPREGNATED MACROPOROUS RESIN [J].
ISSHIKI, K ;
TSUJI, F ;
KUWAMOTO, T ;
NAKAYAMA, E .
ANALYTICAL CHEMISTRY, 1987, 59 (20) :2491-2495
[10]   Recovery of uranium from phosphoric acid solutions using chelating ion-exchange resins [J].
Kabay, N ;
Demircioglu, M ;
Yayli, S ;
Gunay, E ;
Yuksel, M ;
Saglam, M ;
Streat, M .
INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH, 1998, 37 (05) :1983-1990