METHODOLOGY QUANTITATIVE ANALYSIS PROCEDURE THIN SAMPLES: CHARACTERISTIC LINE INTENSITY RELATED TO ELEMENTARY CONCENTRATION BY EQUATION: DETECTION LIMIT.

Apresentação em tema: "METHODOLOGY QUANTITATIVE ANALYSIS PROCEDURE THIN SAMPLES: CHARACTERISTIC LINE INTENSITY RELATED TO ELEMENTARY CONCENTRATION BY EQUATION: DETECTION LIMIT."— Transcrição da apresentação:

1 METHODOLOGY QUANTITATIVE ANALYSIS PROCEDURE THIN SAMPLES: CHARACTERISTIC LINE INTENSITY RELATED TO ELEMENTARY CONCENTRATION BY EQUATION: DETECTION LIMIT LIMITS DETECTION (LMD) WERE CALCULATED USING THE EQUATION: S i : ELEMENTARY SENSIBILITY M D: MATRIX SURFACE DENSITY m i :ELEMENT SURFACE DENSITY I (BG) = BACKGROUND INTENSITY t = EXCITATION TIME X-RAYS SPECTROMETER CALIBRATION EXPERIMENTAL ELEMNTARY SENSIBILITY DETERMINATION - S i EXP OBTAINED BASED ON CHARACTERISTICS LINES INTENSITIES BY SATNDARDS ELEMENTS EXPERIMENTAL ELEMENTARY SENSIBILITY FOR Ti, Mn, Fe, Cu, Zn E Pb SATNDARDS. AtomicElement m i S i EXP Number (Z) ( g/cm -2 ) (cps. cm 2. g -1 ) 22 Ti 43,3 2,57 25 Mn 44,7 6,54 26 Fe 49,4 7,91 29 Cu 42,3 14,71 30 Zn 16,6 17,24 82 Pb 48,3 10,29 OBJECTIVES HEAVY METALS CONTAMINATION EVALUATION FROM LAKES OF SANTA GERTRUDES REGION USE A WEAKLY BONDED METALS EXTRACTION METHOD IN SUSPENDED PARTICULATE MATTER USE OF A COMPLEXATION HEAVY METALS METHOD USE A ENERGY DISPERSIVE X - RAY FLUORESCENCE ANALYTICAL TECHNIQUE SAMPLES PREPARE 100 mL SAMPLE WERE FILTERED IN CELLULOSE ACETATE MEMBRANE (0,45 m) THE FILTER MATERIAL RETAINED WAS SUBMITTED TO FOLLOW TREATMENTS: 1. EXTRACTION PROCEDURE AIMING THE NO - RESIDUAL FRACTION 2. METALS COMPLEXATION PROCEDURE CALIBRATION STANDARDS COMMERCIALLY AVAILABLE STANDARDS (MICROMATTER), CONTAINING THE ELEMENTS Ti, Mn, Fe, Cu, Zn AND Pb. SAMPLING PLACE AND METHOD LAKE A - LAKE B: SURFACE COLLECTING Storage flask LAKE C : DEEPNESS COLLECTING C 0 : SURFACE - C 1 : 4,5 m - C 2 : 9,0 m Ninskin Bottle SAMPLE TREATMENT PROCEDURES EXPERIMENTAL ELEMENTARY SENSIBILITY, OBTAINED BY X - RAY EXCITATION (MO TARGET) SENSIBILITY CURVE IN FUNCTION OF ATOMIC NUMBER. PERMITS THE ELEMENTARY SENSIBILITY OBTAIN OTHERS INTERESTING ANALYTICAL ELEMENTS QUANTITATIVE ANALYSIS ELEM. LMD A B C C o C 1 C 2 Fe5,34 2479,82 5929,80 1077,93 1231,36 2465,01 Co2,70 10,68 30,35 6,16 9,62 10,75 Ni2,67 8,02 42,49 4,93 9,90 14,33 Cu2,53 11,00 12,14 9,86 10,50 15,00 Zn2,49 90,86 127,46 99,90 77,00 100,32 Pb8,02 69,48 151,74 144,30 134,6815 7,65 LMD - DETECTION LIMITS FOR Fe, Co, Ni, Cu, Zn e Pb: VALUES IN g.g -1 HEAVY METALS CONCENTRATION IN SUSPENDED PARTICULATE MATTER COLLETED IN LAKES A - B - C. VALUES IN g.g -1. (AVERAGE OF TWO REPETITIONS) HEAVY METALS CONCENTRATION CONCENTRATION: Fe > Pb > Zn THE ELEMENTS CREASING TENDANCE RELATED TO LAKE DEEPNESS, SENDO MAIS ACENTUADA FOR Fe, Co E Ni. CONCLUSIONS USE X - RAY FLUORESCENCE ASSOCIATED WITH A COMPLEXATION METHOD PERMITS DETERMINE Fe, Co, Ni, Cu, Zn E Pb CONCETRATION EFICIENT PROCEDURE FOR NO - RESIDUAL FRACTION METAL EXTRACTION THE ADOTTEDED PROCEDURE IS APROPRIETATED FOR ENVIROMENT MONITORING STUDIES REFERENCES CARNEIRO, A. E. V. Análise quantitativa do sedimento depositado nas planícies de inundação do rio Solimões/Amazonas, utilizando a técnica de fluorescência de raios X por dispersão de energia. IPEN/USP, São Paulo, Tese de Doutorado, 1995, 232p. CURRIE, L. A. Limits for quantitative detection and quantitative determination, Anal. Chem., v. 40, p. 586-593, 1968. GARDOLINSKI, P. C. F. Extração sequencial de metais em sedimentos e determinação por espectrometria de massa com fonte de plasma induzido (ICP-MS), utilizando o método da diluição isotópica. CENA/USP, Piracicaba, Dissertação de Mestrado, 1998, 74p. GIAUQUE, R. D., GOULDING, F. S., JAKLEVIC, J. M. & PEHL, R. H., Trace element determination with semiconductor detector X-ray spectrometers. Anal. Chem., v. 45, p. 671, 1973. ORLANDO, R. C. Determinação de elementos traços através da análise por ativação neutrônica em sedimentos do rio Piracicaba datados por 210 Pb. CENA/USP, Piracicaba, 1993. 91 p. Dissertação de Mestrado. SIMABUCO, S. M. e NASCIMENTO Filho, V. F. Monitoramento de metais pesados a nível de traços em águas naturais da região de Campinas por fluorescência de raios X com dispersão de energia e excitação radioisotópica. In: III ENCONTRO NACIONAL DE APLICAÇÕES NUCLEARES - ENAN, 1995. Anais. Caxambú: ENAN, 1995, p. 298. TRISDELL, S. E. e BRESLIN, V. T. – Heavy metals in the environment. J.l of Environ. Qual., v. 24, p. 827 - 33, 1995. van GRIEKEN, R. - Preconcentration methods for the analysis of water by X-ray spectrometric techniques. Anal. Chim. Acta, v. 143, p. 3-34, 1982. HEAVY METALS WEAKLY BONDED IN FINE SUSPENDED PARTICULATE MATTER BY ENERGY DISPERSIVE X-RAY FLUORESCENCE AERIA FHOTO FROM LAKES OF SANTA GERTRUDES REGION STUDY AREA CLOSER TO MANY ENAMELED PAVEMENT CERAMIC INDUSTRIES. LAKES RECEIVED INDUSTRIAL WASTE. ANA ELISA SIRITO DE VIVES (1) ; SANDRA MARIA BOSCOLO BRIENZA (2) ; VIRGÍLIO FRANCO DO NASCIMENTO FILHO (3) ; SILVANA MOREIRA SIMABUCO (4) ; (1) Faculdade de Ciências Matemáticas e da Natureza - FCMN/UNIMEP, aesvives@unimep.br (2) Faculdade de Engenharia e Ciências Químicas - FECQ/UNIMEP, sbrienza@unimep.br (3) Laboratório de Instrumentação Nuclear - CENA/USP Departamento de Ciências exatas - ESALQ/USP, virgilio@cena.usp.br (4) Faculdade de Engenharia Civil - FEC/UNICAMP, silvana@fec.unicamp.br