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NEUTRON ACTIVATION ANALYSIS (NAA)
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ANALISIS INSTRUMENTAL KIMIA
PENGGOLONGAN METODE ANALISIS INSTRUMENTAL KIMIA OTHER METHODS SPECTROSCOPY UVi-Vis (Ultra Ungu-Tampak) AAS (Absorpsi) AES (Auger Electron) RAMAN MOESBAUER NMR (Nuclear Magnetic Resonance) FTNMR ESR (Electron Spin Resonance) PHOTOACUSTIC MS (Mass) EIS (Electron Impact) ISS (Ion Scattering) XPS (Xray Photoelectron) UPS (Ultraviolet Photoelectron) THERMOMETRIC METHOD -DTA -DTG ELECTROMETRIC METHOD pH/ISE Potentiometric Titration Voltammetry Polarography (PDV,DME,DPP) Electrogravimetry and Coulometry Conductometry CHROMATOGRAPHY GC LC HPLC Tandem: GC-MS, LC-MS, LC-MS-MS CHEMICAL ANALYSIS OF SURFACES ISS (Ion Scattering Spectrometry) SIMS (Secondary Ion Mass Spectr.) AES (Auger Emission Mass Spectr.) ESCA (Electron Spectroscopy for Chemical Analysis) SPECTROMETRY FLAME EMISSION ATOMIC ABSORPTION XRF NUCLEAR METHOD (,,) MS (MS/MS,ICP-MS,GC-MS, LC-MS,LC-MS-MS, IMS) SPECTROPHOTOMETRY UV-Vis IR FLUORESCENCE PHOSPHORESCENCE RADIOCHEMICAL/ NUCLEAR METHOD: Radioactive Tracer Spectrometry Spectrometry/LSC (Liquid Scintillation Counter) NAA (Neutron Activation Analysis) Mosbauer 13 Maret015
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TEKNIK ANALITIK NUKLIR
PENGUKURAN LANGSUNG RADIOAKTIVITAS (, dan ) PENGUKURAN TIDAK LANGSUNG METODE AKTIVASI -LANGSUNG (prompt): PGNAA, PIXE -KASEP (delayed): NAA, CPAA, PAA -IBA: NRA, PIGE, RBS, PIXE PENAMBAHAN PERUNUT RADIOAKTIF P ENGGUNAAN SUMBER RADIASI -ABSORPSI: Radiasi: , dan neutron -ANALISIS HAMBURAN (scattering) -PENDAR : PENDAR SINAR (XRF) DATA RADIOAKTIVITAS DATA KADAR UNSUR/LOGAM Gambar 1: Skema teknik analisis nuklir (TAN) 13 Maret015
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Keunggulan Analisis Aktivasi Neutron
-Jenis sampel padat, cair, gas -Tidak memerlukan perlakuan kimia -Tidak terkontaminasi -Analisis unsur serentak (Multiunsur) -Memiliki sensifitas & selektivitas tinggi -Mampu menganalisis unsur orde μg, ng -Dll 13 Maret015
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KONSEP ANALISIS AKTIVASI NEUTRON (AAN) PGNAA NAA 13 Maret015
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NEUTRON ACTIVATION ANALYSIS
For neutron induced reactions VC=0 It enters all nuclei and binds to it. CN is in excited state. PGAA A+1X NAA A+1Y Z+1 NEUTRON INTERACTION OFTEN PRODUCES RADIOISOTOPES : ENTIRE PERIODIC TABLE CHARACTERISTIC RADIATIONS, e.g., GAMMA RAYS ARE MEASURED : CONCN. OF ISOTOPES (ELEMENTS) 13 Maret015
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Although there are several types of neutron sources (reactors, accelerators, and radioisotopic neutron emitters) one can use for NAA, nuclear reactors with their high fluxes of neutrons from uranium fission offer the highest available sensitivities for most elements. Different types of reactors and different positions within a reactor can vary considerably with regard to their neutron energy distributions and fluxes due to the materials used to moderate (or reduce the energies of) the primary fission neutrons. However, as shown in Figure 2, most neutron energy distributions are quite broad and consist of three principal components (thermal, epithermal, and fast). Neutrons Figure 2: A typical reactor neutron energy spectrum showing the various components used to describe the neutron energy regions. 13 Maret015
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The Kartini Facilities
TRIGA Mark II Reactor (100 kW) Neutron Radiography (in experient) Thermal Neutron Activation Analysis Fast Neutron Activation Analysis (14 MeV in experient) Prompt Gamma Activation Analysis (in experient) Spectroscopy (a, b, and g) Radiation Handling Areas Computational Capabilities : AccuSpec, Shampo, Maestro and Genie software Gamma Detector: NaI(Tl), HPGe, Ge(Li) 13 Maret015
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Activation method delayed (AAN) REAKTOR KARTINI Spektrometer
Sistem iradiasi dg rabit system/pneumatic Activation method delayed (AAN) REAKTOR KARTINI TRIGA MARK II, 100 kW Spektrometer 13 Maret015
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TERAS REAKTOR KARTINI TIDAK BEROPERASI
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TERAS REAKTOR KARTINI SAAT BEROPERASI
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TOTAL ELEMENTS AMENABLE TO NAA > 70
FNAA S Limit Deteksi dalam ppb (10-9) CONV. NAA and PGNAA : DL ppb 13 Maret015
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DEPENDS ON FLUX, DETECTION EFFICIENCY AND IRRADIATION TIME
DETECTION LIMITS DEPENDS ON FLUX, DETECTION EFFICIENCY AND IRRADIATION TIME ELEMENT DETECTION LIMIT [g] In, Eu, Dy 10-13 to 10-12 Mn, Lu 10-12 to 10-11 Co, Br, I, Sm, Ho, Hf, Re, Ir, Au, Th, U 10-11 to 10-10 Na, Cl, Cu, Ga, Ge, Se, As, Pd Sb, Te, Yb, Ta, W, Pt 10-10 to 10-9 K, Sc, Ni, Rb, Sr, Y, Nb, Ru, Cd Sn, Gd, Tb, Tm, Os, Hg 10-8 to 10-9 * CALCULATED USING A NEUTRON FLUX OF 1013n/SEC/Cm2 & A 20% RELATIVE EFFICIENCY DETECTOR 13 Maret015
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Perbandingan Limit Deteksi berbagai Metode
METODE LIMIT DETESI AAS – 10-9 g AES – 10-7 g FLAME EMISSION – 10-9 g ANODIC STRIPP. VOLTAMETRY – 10-9 g MASS SPECTROMETRY g ICP-MS g GAS CHROMATOGRAPHY – 10-7 g XRF – 10-7 g NAA – g IBA – 10-9 g 13 Maret015
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14 MeV-NAA : FNAA (Fast Neutron)
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14 MeV-NAA : FNAA NEUTRON GENERATOR : Cockroft-Walton accelerator principle NEUTRONS OF ~14 MeV FROM t(d,n) RXN AVAILABLE FLUX: 109 n.cm-2.s-1 from a neutron yield of 2.5x1011 n.s-1 Threshold reactions:(n,p), (n,2n), (n,) etc. Inelastic scattering rxns (n,n’): C, O and N (200, 100 and ~20 mb respectively) Determination of many elements including C, N and O possible Important tool for detection of explosives (TNT, RDX etc.): high C, N, O high N/O and/or C/O ratio 13 Maret015
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14 MeV-NAA : FNAA Element Nuclear Reaction Product Half-life
Gamma-ray (keV) O 16O (n, p) 16N 7.13 s 6130, 7120 N 14N (n, 2n) 13N 9.97 min 511 F 29F (n, p) 19O 30 s 197.4 Mg 24Mg (n, p) 24Na 15 h 1368.5 Si 28Si (n, p) 28Al 2.24 min 1779 P 31P (n, ) 28Al Fe 56Fe (n, p) 56Mn 2.58 h 847 Cu 63Cu (n, 2n) 62Cu 10 min Zn 64Zn (n, p) 64Cu 12.8 h Zr 90Zr (n, 2n) 89mZr 4.18 min 588 Th Fission - Delayed neutron U 13 Maret015
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PROMPT GAMMA-RAY NAA: PGNAA
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It is complementary to conventional NAA
PGNAA is an online technique : Measurement of capture gamma rays after neutron absorption It is complementary to conventional NAA Analysis of low Z elements (H, B, C, N, Si, P,S): Best for H and B analysis Determination of many elements including Hg, Cd, Sm & Gd The k0-based PGNAA: Advantageous PGAA WORK INVOLVED SETTING UP OF A SYSTEM: DETECTION & SHIELDING CHARACTERISATION OF THE NEUTRON BEAM EFFICIENCY DETERMINATION (~ MeV) DETERMINATION OF PROMPT k0-FACTORS ANALYTICAL APPLICATION 13 Maret015
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Ability to determine light elements (H,B,N,C,P,S,Si)
Some important features of PGNAA Ability to determine light elements (H,B,N,C,P,S,Si) Analysis of biological sample Ability to determine toxic elements (Cd, Hg) with high sensitivity Environmental samples Nondestructive multielemental bulk analysis Flexibility of sample size and shape Archeological, geo- and cosmo- chemical samples Isotopic analysis is possible (S,Si,Ni) 13 Maret015
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Schematic representation of the PGNAA set up
Neutron beam line Lead shield Boron Carbide HPGe detector Beam Dump Sample Holder Schematic representation of the PGNAA set up BGO shield 13 Maret015
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WORK SETTING UP PGNAA SYSTEM CALIBRATION & CHARACTERISATION k0 FACTORS
BACKGROUND PROBLEMS CAPTURE GAMMA RAYS IN 60Co APPLICATIONS A) ANALYSIS OF SAMPLES CONTAINING B,Cd,Gd,Hg B) ANALYSIS OF A FEW CRMS C) ANALYSIS OF METEORITES D) ANALYSIS OF SS ALLOYS JRNC 250 (2001) 303, NIMA 457 (2001) 180 NIM A 516(2004)143, ANAL CHIM ACTA ( COMM), ANAL CHEM ( PREP) 13 Maret015
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Elemental densities and ratios of three classes of substances
C/O C/N Cl/O Plastics M-H H-L M M-N VH - Narcotics L H, >3 Explosives L-M L, <1 L – Low, M – Medium, H – High, VH- Very high 13 Maret015
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METODE AAN 13 Maret015
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NAA-Kay zero (in experient)
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R & D WORK ON NAA Collaborations NAA Development of Methodologies:
APPLICATIONS Reference materials, Ruby, Emerald, Sediment, Leaf, Cereal, Mn-Nodules Serpentines, Zircaloy, SS, Aluminium, Meteorites Collaborations Chemical NAA, Radiochemical NAA Speciation NAA NAA Development of Methodologies: k0-BASED INTERNAL MONO STANDARD NAA IN-SITU REL-EFFICIENCY LSNAA STANDARD-LESS NAA k0-BASED NAA SINGLE COMPARATOR: Au DETMN: f , & k0 VALIDATION: CRMs k0-BASED PGNAA EFFICIENCY k0-FACTORS APPLICATIONS 13 Maret015
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RADIOACTIVITY IN ENVIRONMENT
RADIOACTIVITY MEASUREMENT RADIOACTIVITY IN ENVIRONMENT 1. ESSENTIALLY NATURAL PROCESSES, e.g., RADON & DP 2. ANTHROPOGENIC : MINING, PROCESSING, REPROCESSING DIAGNOSTIC, TESTING, ACCIDENTS AS ON NOW FIRST IS MUCH MORE RADIOACTIVITY MEASUREMENTS : , , LARGE SAMPLES OF SOIL, WATER; AIR PARTICULATES COLLECTED ON FILTERS; FOOD STUFFS CHEMICAL PRECONCENTRATION 13 Maret015
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Toxicity depends on species The five major species:
SPECIES OF ARSENIC Toxicity depends on species The five major species: As(III), As(V), MMA, DMA and AsB In natural water two major species: As(III) & As(V) Drinking water limit (As): 10 ng.mL-1 (WHO) ARSENIC SPECIES: WATER SYSTEM Standardized two chemical separation methods: Ion exchange separation Solvent extraction 13 Maret015
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INORGANIC ARSENIC SPECIATION : Dowex 1X8 in acetate form
TOTAL ARSENIC IN DRINKING WATER BY INAA: ng.mL-1 in samples from Kolkata city INORGANIC ARSENIC SPECIATION : Dowex 1X8 in acetate form As(III)+As(V) IN 8M AcOH 0.12M HCl As(V) PERCENT RECOVERIES OF ARSENIC SPECIES QUANTITATIVE (96-100%) IN BOTH ION EXCHANGE AND SOLVENT EXTRACTION METHODS SOLV.EXT.: APDC-MIBK IN pH 1-5.5 As(V) As(V) As(III) 13 Maret015
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TERIMA KASIH 13 Maret015
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