13 maret015aguszani@batan.go.id1 neutron activation analysis (naa)

13 Maret015 aguszani@batan.go.id 1

NEUTRON ACTIVATION ANALYSIS (NAA)

SPECTROSCOPYUVi-Vis (Ultra Ungu-Tampak)AAS (Absorpsi)AES (Auger Electron)RAMANMOESBAUERNMR (Nuclear Magnetic Resonance)FTNMRESR (Electron Spin Resonance)PHOTOACUSTICMS (Mass)EIS (Electron Impact)ISS (Ion Scattering)XPS (Xray Photoelectron)UPS (Ultraviolet Photoelectron)

SPECTROPHOTOMETRYUV-VisIRFLUORESCENCEPHOSPHORESCENCE

RADIOCHEMICAL/ NUCLEAR METHOD:Radioactive Tracer SpectrometrySpectrometry/LSC (Liquid Scintillation Counter)NAA (Neutron Activation Analysis)Mosbauer

THERMOMETRIC METHOD-DTA-DTG

OTHER METHODS

SPECTROMETRYFLAME EMISSIONATOMIC ABSORPTIONXRFNUCLEAR METHOD (,,)MS (MS/MS,ICP-MS,GC-MS,LC-MS,LC-MS-MS, IMS)

CHROMATOGRAPHYGCLCHPLCTandem: GC-MS, LC-MS, LC-MS-MS

ELECTROMETRIC METHODpH/ISEPotentiometric TitrationVoltammetryPolarography (PDV,DME,DPP)Electrogravimetry and CoulometryConductometry

CHEMICAL ANALYSIS OF SURFACESISS (Ion Scattering Spectrometry)SIMS (Secondary Ion Mass Spectr.)AES (Auger Emission Mass Spectr.)ESCA (Electron Spectroscopy for Chemical Analysis)

PENGGOLONGAN METODEANALISIS INSTRUMENTAL KIMIA

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TEKNIK ANALITIK NUKLIR

PENGUKURAN LANGSUNGRADIOAKTIVITAS

(, dan )

PENGUKURAN TIDAK LANGSUNGMETODE 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)

Gambar 1: Skema teknik analisis nuklir (TAN)

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DATA RADIOAKTIVITAS

DATA KADAR UNSUR/LOGAM

-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

Keunggulan Analisis Aktivasi Neutron

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ANALISIS AKTIVASI NEUTRON (AAN)

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KONSEP

NAA

PGNAA

NEUTRON ACTIVATION ANALYSIS

A+1X

A+1YZ+1

XAZ

NEUTRON INTERACTION OFTEN PRODUCES RADIOISOTOPES : ENTIRE PERIODIC TABLE

CHARACTERISTIC RADIATIONS, e.g., GAMMA RAYS ARE MEASURED : CONCN. OF ISOTOPES (ELEMENTS)

NAA

PGAA

• For neutron induced reactions

VC=0

• It enters all nuclei and binds to it.

• CN is in excited state.

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Figure 2: A typical reactor neutron energy spectrum showing the various components used to describe the neutron energy regions.

• 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

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Slide#8

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)

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Sistem iradiasi dg rabit system/pneumaticREAKTOR KARTINI

REAKTOR KARTINITRIGA MARK II, 100 kW

Spektrometer 13 Maret015 9aguszani@batan.go.id

Activation methoddelayed (AAN)

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TERAS REAKTOR KARTINI TIDAK BEROPERASI

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TERAS REAKTOR KARTINI SAAT BEROPERASI

TOTAL ELEMENTS AMENABLE TO NAA > 70

FNAA

S

CONV. NAA and PGNAA : DL 0.01-1000 ppb13 Maret01512aguszani@batan.go.id

Limit Deteksi dalam ppb (10-9)

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, PdSb, 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

DETECTION LIMITS DEPENDS ON FLUX, DETECTION EFFICIENCY AND IRRADIATION TIME

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Perbandingan Limit Deteksi berbagai Metode

METODE LIMIT DETESI

AAS 10-6 – 10-9 gAES 10-6 – 10-7 gFLAME EMISSION 10-6 – 10-9 gANODIC STRIPP. VOLTAMETRY 10-8 – 10-9 gMASS SPECTROMETRY 10-6 gICP-MS 10-9 gGAS CHROMATOGRAPHY 10-6 – 10-7 gXRF 10-5 – 10-7 gNAA 10-5 – 10-10 gIBA 10-6 – 10-9 g

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14 MeV-NAA : FNAA (Fast Neutron)

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14 MeV-NAA : FNAANEUTRON 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

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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 2.24 min 1779

Fe 56Fe (n, p) 56Mn 2.58 h 847

Cu 63Cu (n, 2n) 62Cu 10 min 511

Zn 64Zn (n, p) 64Cu 12.8 h 511

Zr 90Zr (n, 2n) 89mZr 4.18 min 588

Th Fission - Delayed neutron

U Fission - Delayed neutron

14 MeV-NAA : FNAA

PROMPT GAMMA-RAY NAA: PGNAA

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PGAA WORK INVOLVED

SETTING UP OF A SYSTEM: DETECTION & SHIELDINGCHARACTERISATION OF THE NEUTRON BEAMEFFICIENCY DETERMINATION (~ 0.1-10 MeV) DETERMINATION OF PROMPT k0-FACTORSANALYTICAL APPLICATION

PGNAA is an online technique : Measurement of capture gamma rays after neutron absorption

1. It is complementary to conventional NAA2. Analysis of low Z elements (H, B, C, N, Si, P,S):

Best for H and B analysis3. Determination of many elements including Hg, Cd,

Sm & Gd

The k0-based PGNAA: Advantageous

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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)

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Neutron beam line

Lead shield

Boron CarbideHPGe

detector

Beam Dump

Sample Holder

Schematic representation of the PGNAA set up

BGO shield

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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) 180NIM A 516(2004)143, ANAL CHIM ACTA ( COMM), ANAL CHEM ( PREP)13 Maret015 22aguszani@batan.go.id

Substance H C N O Cl C/O C/N Cl/O

Plastics M-H H H-L M M-N M VH -

Narcotics H H L L M H, >3 H VH

Explosives L-M M H VH M-N L, <1 L, <1 L-M

L – Low, M – Medium, H – High, VH- Very high

Elemental densities and ratios of three classes of substances

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METODE

AAN

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aguszani@batan.go.id

NAA-Kay zero(in experient)

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NAA

k0-BASED NAASINGLE COMPARATOR: Au

DETMN: f , & k0

VALIDATION: CRMs

k0-BASEDINTERNAL MONO STANDARD NAA

IN-SITU REL-EFFICIENCYLSNAA

STANDARD-LESS NAA

k0-BASED PGNAA

EFFICIENCYk0-FACTORS

APPLICATIONS

APPLICATIONSReference materials,

Ruby, Emerald, Sediment,Leaf, Cereal, Mn-NodulesSerpentines, Zircaloy, SS,

Aluminium, Meteorites

Chemical NAA, Radiochemical NAA

Speciation NAA

R & D WORK ON NAA

Collaborations

Development ofMethodologies:

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RADIOACTIVITY MEASUREMENT

RADIOACTIVITY IN ENVIRONMENT1. ESSENTIALLY NATURAL PROCESSES, e.g., RADON & DP2. 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

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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)

SPECIES OF ARSENIC

ARSENIC SPECIES:WATER SYSTEM

Standardized two chemical separation methods:

(i) Ion exchange separation(ii) Solvent extraction

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INORGANIC ARSENIC SPECIATION: Dowex 1X8 in acetate form

As(V)

As(V)

As(V)

As(III)+As(V)IN 8M AcOH 0.12M HCl

As(III)

TOTAL ARSENIC IN DRINKING WATER BY INAA: 20-650 ng.mL-1 in samples from Kolkata city

• 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

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TERIMA KASIH

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