ENVIRONMENTAL SAMPLES ANALYSIS BY ATOMIC ABSORPTION SPECTROMETRY (AAS) AND INDUCTIVELY COUPLED PLASMA-OPTICAL EMISSION SPECTROSCOPY (ICP-AES)

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1 ENVIRONMENTAL SAMPLES ANALYSIS BY ATOMIC ABSORPTION SPECTROMETRY (AAS) AND INDUCTIVELY COUPLED PLASMA-OPTICAL EMISSION SPECTROSCOPY (ICP-AES) I. V. POPESCU 1,2,3, C. STIHI 1, GH. V. CIMPOCA 1,2, G. DIMA 1, GH. VLAICU 4, A. GHEBOIANU 2, I. BANCUTA 2, V. GHISA 5, G. STATE 6 1 Valahia University of Târgoviºte, Multidisciplinary Research Institute for Science and Technologies, No. 2, Carol I Street, Târgoviºte, Romania, ivpopes@yahoo.com 2 Academy of Romanian Science 3 Horia Hulubei Institute of Physics and Nuclear Engineering, Bucharest Mãgurele, Romania 4 Special Steel Complex, Physics Laboratories, Târgoviºte, Romania 5 Ovidius High School, Constanþa 6 Enãchiþã Vãcãrescu High School, Târgoviºte, Romania Received October 10, 2008 Biological samples are interested from many aspects of environmental monitoring. Starting from assumption that the pollution factor from environmental can modify the normal concentration of elements in biological samples, we decided to control the presence of toxic elements and the deviation from their normal concentration. The aim of this work is to determine the elemental composition of some tree leaves situated in the vicinity of an industrial pollution source Special Steel Trust Târgoviºte. Also, by this work we analyzed surface water from Ialomiþa River from Dâmboviþa County. We try to demonstrate the applicability of different atomic methods, like AAS and ICP-AES, for environmental monitoring of Dâmboviþa County. Key words: AAS, ICP-OES, leaves trees, Ialomiþa River. 1. INTRODUCTION Environmental pollution remains are important issue for population, economic and political decision factors in all countries. The small territory of Romania is affected by pollutants from different pollution sources: chemical industries, iron and steel smelter, coal mining and thermal power stations, cement factories, auto traffic, the use of pesticides and fertilizer, so, it is vital to know the elemental concentration of heavy and toxic elements in flora and fauna and to quantify these using analytical methods. Paper presented at the National Conference of Physics, September, 2008, Bucharest Mãgurele, Romania. Rom. Journ. Phys., Vol. 54, Nos. 7 8, P , Bucharest, 2009

2 742 I. V. Popescu et al. 2 In Dambovita zone, the main polluting regional industries are: stainless steel works, Special Steel Trust Târgoviºte, cement and related materials production (Fieni), glass and lighting sources production (Târgoviºte, Fieni), chemicals materials production (Târgoviºte, Doiceºti), coal mining and thermal power station (Doiceºti), oil exploration (Târgoviºte, Moreni, Gãieºti). Using the methods of absorption and emission spectroscopy were studied the concentration of elements in some tree leaves samples collected near Special Steel Trust Târgoviºte and surface water samples from Ialomiþa River. The Atomic Absorption Spectrometry (AAS) [1] is the most widely utilized method today for rapid and quantitative elemental analysis. The detection limit in AAS analysis method is up to 0.1 μg/kg under optimum test conditions. A material sample, in a liquid solution, is atomized through rapid heat application and placed in the radiation path of several element-specific light source. The sample atoms absorb ultraviolet or visible light and make transitions to higher electronic energy levels. The analyte concentration is determined from the amount of light absorption. The atomic density determine the absorption rate and the Lambert-Beer s law give the value of absorbance from each element of the sample which is proportional with the concentration of that element. The Lambert-Beer law is difficult to applying directly in AAS due to variations in the atomization efficiency from the sample matrix, and nonuniformity of concentration and path length of analyte atoms (in graphite furnace AA). The high sensitivity by AAS is obtained using the relative analysis method. The ICP-AES is an emission spectrometric technique [2, 3], exploiting the fact that excited electrons emit energy at a given wavelength as they return to ground state. The fundamental characteristic of this process is that each element emits light at wavelengths peculiar to its chemical character. The intensity of the light emitted at the chosen wavelength is proportional to the concentration of that element in the analyzed sample. ICP-AES is a fast and high sensitivity (ppb-ppm) multielemental analytical technique which can be applied to a wide range of sample types: metals, archaeological, biological, and medical samples, environmental samples (water streams, airborborne particles and coal fly ash, etc.). The sample analyzed must be in solution. 2. EXPERIMENTAL The atomic absorption spectrometer used by us is an AAS AVANTA GBC with hallow cathode lamp (HCL). The emission spectroscopy analysis were performed using the Baird ICP 2070 Sequential Plasma Spectrometer which consists of a sample introduction system, a plasma torch, a plasma power supply and an optical measurement system.

3 3 Environmental samples analysis 743 Samples: The samples analyzed by AAS and ICP-AES methods were leaves of different trees: walnut (P1, P2) and apple tree (P3, P4) collected from ten points of different distances from pollution source, Special Steel Trust, Târgoviºte (Table 1). The leaves samples analyzed by AAS experiments were prepared in the following manner: leaves of trees, collected of approximately in some position, have been dried at a temperature of 105 C in a clean box preventing further contamination. The dried leaves have been grained and after powdering 0.25 g powder leaves was digested in 8 ml nitric acid and 10 ml peroxide. After digestion each solution sample was filtrated and diluted with 50 ml volume of deionized water. Table 1 Type of samples Sample code Type of sample Collecting point P1 (two samples) Leave of walnut (two samples) 2 km distance of pollution source P2 (two samples) Leave of walnut (two samples) 5 km distance of pollution source P3 (three samples) Leave of apple (three samples) 2 km distance of pollution source P4 (three samples) Leave of apple (three samples) 5 km distance of pollution source In ICP-AES measurements were analyzed the same leaves samples prepared in the following manner: after powdering, dry 0.25 g powder leaves were digested in 5 ml nitric acid. For a good digestion 10 ml perchloric acid have been added together with 1 ml HCl. The cooled solution was diluted with deionized water up to 100 ml solution. The surface water samples were collected from Ialomiþa River (21 collecting points). The samples is accurately weighed and then dissolved, often using strong nitric acid. The resulting solution was diluted with deionized water up to 100 ml solution. 3. RESULTS AND DISCUSSIONS Leaves of trees samples: The collected samples were analyzed by AAS method at Atomic Absorption Spectrometry Laboratory of Valahia University of Târgoviºte. The mean value of concentrations obtained is given in Table 2 for elements: Cd, Co, Cu, Cr, Fe, Mn, Zn and Se. In the same samples, the mean value Ca, Mg and Sr concentrations determined by ICP-AES technique are given in Table 3. The concentration values of Cu, Cr, Fe and Mn contained in samples (Table 2) are slowly decreasing with the distance to pollution source. The concentrations of Zn and Se (Table 2), Ca and Mg (Table 3) have for the same samples, in the statistical limits, constant values. The concentration of Cd was

4 744 I. V. Popescu et al. 4 Table 2 The mean value of elemental concentrations (mg/kg) in dry leaves tree samples obtained by AAS method Sample Cd Co Cu Cr Fe Mn Zn Se P P P P Standard error between 3 5%. Table 3 The value of elemental concentrations (mg/kg) in dry leaves tree samples determined by ICP-AES method Sample Ca Mg Sr P P P P Standard error between 3 5%. detected in P1 and P3 samples collected at 2 km away of pollution source and Sr was determined only in P1 sample. Water samples of Ialomiþa River: The concentrations of Fe, Mn and Zn from surface water samples of Ialomiþa River determined by AAS method are given in Table 4, with an instrumental error between 3 5%. Standard values of surface water for class 1, 2 and 3 are presented in the Table 5 which means: class 1 very clean fresh surface water, ecosystem consummation where basic organisms can breed naturally, resources used for consumption which requires ordinary water treatment processes before use; aquatic organism of conservation, fisheries an recreation; class 2 medium clean fresh surface water sources used for: consumption, but passing through and ordinary treatment process before use and agriculture; fairly clean fresh surface water resources used for consumption which requires special water; treatment process before use and industry [4, 5, 7]. Natural water quality problems are caused mainly by Fe, Mn, Zn and hydrogen sulphite and hardness [6]. When the water quality is investigated, certain parameters can be used to indicate possible contamination: electrical conductivity and chemical elements, for instance: K, Cl, S, Fe, Mn, Zn, Ni, Cd, Cr, Pb and so on. We can see (Table 4) that, there are important increases of Fe, Mn and Zn concentrations after the passes of the river from Târgoviºte city, which is an impor-

5 5 Environmental samples analysis 745 Table 4 Fe, Mn and Zn concentrations on Ialomiþa River in different collecting points Collecting points Fe [mg/l] Mn [mg/l] Zn [mg/l] Moroieni aval Moroieni amonte Pietroºiþa aval Pietroºiþa amonte Fieni aval Fieni amonte Pucioasa aval Pucioasa amonte Braneºti aval Doiceºti aval Doiceºti amonte Târgoviºte aval Târgoviºte amonte Comiºani aval Comiºani amonte Bilciureºti aval Bilciureºti amonte Dobra aval Dobra amonte Bãleni aval Bãleni amonte Table 5 Standard values of surface water for Class1, 2 and 3 Element Class 1 [mg/l] Class 2 [mg/l] Class 3 [mg/l] Ca Fe Cu Ni Mn Zn Cd Cr Pb Na tant industrial center of Romania. The present recommended limits for Fe, Mn and Zn in water are respectively 0.3 mg/l, 0.1 mg/l and 0.03 mg/l (Table 5).

6 746 I. V. Popescu et al. 6 Water with a high Fe, Mn and Zn content is not considered a health problem, but it can be very objectionable in taste, odor and appearance. 4. CONCLUSIONS In summary the AAS and ICP-AES analysis methods give the possibility to determine the elemental composition of environmental samples (flora and fauna) with a great sensibility. High precision measurements [1 3, 7] of the physical-chemical environmental factors are essential but not sufficient to assess the response of ecosystems to stress. A main goal of environmental monitoring is to monitories the state of whole ecosystems using bioindicators. REFERENCES 1. Michael B. Sperling, Bernhard Welz, Atomic Absorbtion Spectroscopy, Weinheim, Wiley-VCH. ISBN R. W. J. M. Boumans, Inductively Coupled Plasma Emission Spectroscopy, John Wiley & Sons, New York, M. Tatro, Optical Emission Inductively Coupled Plasma in Environmental Analysis, Encyclopedia of Analytical Chemistry, ISBN B. R. Davies, K. F. Walker, The ecology of river systems, 1986, John Wiley & Sons, New York, H. M. Dix, 1981, Environmental Pollution, John Wiley, Chichester, J. Koski-Vahala, H. Hartikainen, P. Tallberg, Journal of Environmental Quality 30: (2001). 7. Simona Apostol, Claudia Stihi, Cãlin Oros, The use of the chlorophyll fluorescence for estimation of photosynthetic electron transport flow in water stressed pea plants, Journal of Optoelectronics and Advanced Materials, 9, 9, pp , 2007.

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