aplikasi teknik nuklir bidang kimia

Aplikasi Teknik Nuklir Bid Ki iBidang Kimia

Pusat Pendidikan dan PelatihanBadan Tenaga Nuklir Nasional

Latar Belakangg

• Perkembangan Teknologi Nuklir :• Industri• Kedokteran• Lingkungan

D k bid R di ki i• Dukungan bidang Radiokimia

TujuanTujuanPeserta bisa menjelaskan Aplikasi Teknik Nuklir d l Bid Ki idalam Bidang KimiaKhusus :

– Menjelaskan prinsip AAN– Menjelaskan prinsip Teknik Pengenceran Isotop

– Menjelaskan prinsip Titrasi Radiometri– Menjelaskan prinsip nuclear dating– Menjelaskan aplikasi untuk analisis

radioaktivitas lingkungan

SistematikaSistematika

• Bab I : Pendahuluan• Bab II : Analisis Unsur

1. Analisis Aktivasi Neutron2. Teknik Pengenceran Isotop3. Titrasi Radiometri

• Bab III : Nuclear Dating• Bab IV : Analisis Radioaktivitas LIngkungan

Bab IIAnalisis UnsurAnalisis Unsur

Prinsip AANPrinsip AAN

Formulasi AktivasiFormulasi Aktivasi

R = . .N

irteNA 1 eNA 1

irtAv eM

mNA 1

Proses Aktivasi dan PeluruhanProses Aktivasi dan Peluruhan

Tampang Lintang T k N t Th lTangkapan Neutron Thermal

Target (n,) Target (n,)23Na 0,4 63Cu 4.526Mg 0.038 75As 4.327Al 0.23 81Br 2.437Cl 0.43 109Ag 9148Ca 1 09 139La 8 948Ca 1.09 139La 8.951V 4.9 152Sm 206

50Cr 15.9 151Eu 920055Mn 13.3 186W 37.958Fe 1.28 191Ir 95459Co 37.2 197Au 98.7

Metode AAN

• Metode Absolut• Metode Komparator Tunggal• Metode Komparator Tunggal• Metode Relatif• Metode ko

Spektrum GammaSpektrum Gamma

Sensitivitas / Limit DeteksiSensitivitas / Limit DeteksiSensitivitas picograms Elementsg

1 Dy, Eu

1 - 10 In, Lu, Mn

10 - 100 Au, Ho, Ir, Re, Sm, W

100 - 1E3 Ag, Ar, As, Br, Cl, Co, Cs, Cu, Er, Ga, Hf, I, La, Sb, Sc, Se, Ta, Tb, Th, Tm, U, V, Yb

1E3 - 1E4Al, Ba, Cd, Ce, Cr, Hg, Kr, Gd, Ge, Mo, Na, Nd, Ni, Os, Pd, Rb, Rh Ru Sr Te Zn ZrRh, Ru, Sr, Te, Zn, Zr

1E4 - 1E5 Bi, Ca, K, Mg, P, Pt, Si, Sn, Ti, Tl, Xe, Y

1E5 - 1E6 F, Fe, Nb, Ne1E5 1E6 F, Fe, Nb, Ne

1E7 Pb, S

Aplikasi AANAplikasi AAN• Lingkungan :

– Analsis Pencemaran logam berat– Pemetaan Geokimia

K h t• Kesehatan :– Analisis logam berat dalam makanan dan jaringan

P liti d l b b t kit– Penelitian dalam pengembangan pengobatan penyakit

• Pangan : kandungan unsur mikro dalam bahan makanan

• Industri : – kualitas batu bara, – batuan dalam sumur

Teknik Pengenceran Isotop (TPI)Teknik Pengenceran Isotop (TPI)

• pekat encer 'S• pekat encerpengenceran

1''

SSmm

• Radioisotop : memancarkan radiasi, mudah diukur

m’ = massa/volume zat radioaktifm massa/volume zat radioaktifm = massa/volume bahan yang dianalisisS’ = aktivitas jenis zat radioaktifS = aktivitas jenis setelah pengenceranj p g

Aplikasi TPIAplikasi TPI

• Pengukuran Volume fluida di dalam tanahPengukuran Volume fluida di dalam tanah• Kedokteran Nuklir

A li i K tit tif U• Analisis Kuantitatif Unsur

Titrasi RadiometriTitrasi Radiometri• Merupakan analisis kuantitatif• Seperti titrasi biasa tetapi senyawa hasil mudah• Seperti titrasi biasa, tetapi senyawa hasil mudah

dipisahkan• Titik akhir titrasi ditunjukkan oleh perubahan aktivitas

secara mencolok

Volume Volume

Bab IIINuclear DatingNuclear Dating

Prinsip Nuclear DatingPrinsip Nuclear Dating

•Umur batuan : 238U/206Pb

•Tidak mengandung uranium : 40K/40Ar40K + 1e

40Ar (t1/2=13 109 tahun)K + -1e Ar (t1/2 1,3 . 10 tahun )

Material yang berasal dari makhluk hidup : 14C/12C

Preparasi Radiokimia untuk Analisis Radioaktivitas LingkunganAnalisis Radioaktivitas Lingkungan

1. Analisis137Cs dalam Sampel Air Laut2. Analisis 222Rn dalam Sampel Airp3. Analsis U dan Pu dalam Sampel

TanahTanah4. Analisis 90Sr dalam Sampel

LingkunganLingkungan

Radiochemical Preparation for Analysis of 137Cs in Seawaterfor Analysis of Cs in Seawater

• Average Activity 2 Bq/m3Average Activity 2 Bq/m• Sample volume : 20 L• Radioactivity Measurement by GammaRadioactivity Measurement by Gamma

Spectrometer• The purpose of preparation :• The purpose of preparation :

• to collect Cs from a large sample size• to avoid self-absorptionto avoid self absorption • to make easier in radioactivity measurement

Radiochemical Preparation for Analysis of 137Cs in Seawater

Seawater 5 L

for Analysis of Cs in Seawater

Seawater 5 LAdd 100 mL of 3 M HCl for washing the containerAdd Cs carrier, 2 gr AMPStir for 30 minutesSt d th 12 hStand more than 12 hoursDecantationFilterFilter

precipitate* supernatant liquid**precipitate supernatant liquid

Radiochemical Preparation for Analysis of 137Cs in Seawater

precipitate*

y

precipitate

Add 2 M HClAdd 2 M HCl(for washing)

precipitate (MnO2)precipitate (MnO2)mix

G S t tGamma Spectrometry

supernatant liquid**p qAdjust pH 8.0-8.5 with NH4OHAdd 10 g MnO powderAdd 10 g MnO2 powderStir for 30 minutesStand for more 12 hoursStand for more 12 hoursDecantationFilterFilter

precipitate supernatantmix

Preparasi Radiokimia t k A li i 222R d l S l Aiuntuk Analisis 222Rn dalam Sampel Air

S l iSampel air

+ xyleney

Ekstraksi

Fasa organik

+ SintilatorPengukuran dengan LSC

+ Sintilator

Radiochemical Preparation for Analysis of Actinides ( U and Pu) in Soilof Actinides ( U and Pu) in Soil

U PuU Pu

Activity Level 0.2 mg/Kg 40 mBq/Kg

S l 10 50

• Radioactivity Measurement by Alpha

Sample mass 10 g 50 g

• Radioactivity Measurement by Alpha SpectrometerTh f ti• The purpose of preparation :

• to avoid self-absorption • to separate other radionuclides

Radiochemical Preparation for Analysis of Pu in Soilfor Analysis of Pu in Soil

Pretreatment

Solvent Extraction Ion Exchange

Preparation for ElectrodepositionPreparation for Electrodeposition

ElectrodepositionElectrodeposition


P t t tPretreatmentSoil

Heat at 105oC for 2 hoursHeat at 500oC for 4 hoursAdd 242Pu standard solutionAdd 242Pu standard solutionAdd 8 M HNO3Filter

Residue FiltrateResidue Filtrate

Radiochemical Preparation for Analysis of Pu in Soil

Purification by Solvent ExtractionFiltrateFiltrate

Add TOA-xyleneExtract

Add 8 M HNO aqAdd 8 M HNO3Extract

Add 10 M HCl

org

org aqAdd 10 M HClExtract

org aqAdd NH4I.HCl orgExtract

aq Add XyleneExtractorg

aqorg aq


Purification by Ion Exchange8 M HNO

Filtrate8 M HNO3

10 M HCl

NH4I.HCl4 C

Anion ColumDowex 1-X8, 100-200 mesh100 200 mesh

Eluent


Preparation for Electrodeposition

Eluent(NH4I.HCl)

Heat to dry

Dissolve by 2 M H2SO4Add h l d

residue

Add methylred

solution (red)Add NH OH until pH 4Add NH4OH until pH 4

solution (yellow)Add 2 M H2SO4 until pH 22 4 p

solution (red)


Electrodeposition

Pt anodesolution (red)

0.5 Ampere, 2 hoursAdd NH4OH

Stainless steel cathode

Radiochemical Preparation for Analysis of 90SrAnalysis of 90Sr

• Radioactivity Measurement through 90Y by β• Radioactivity Measurement through 90Y by βCounter (Low Backgroud Counter)

• The purpose of preparation :• The purpose of preparation :• To separate from other radionuclides

t i l t 90Y• to isolate 90Y

Radiochemical Preparation for Analysis of 90Srfor Analysis of Sr

Pretreatment

Separation of Sr from Ca by Nitrate Precipitation

Scavenging to Separate Sr from existing Y

Determination of Chemical Recovery for Sr

Milking of 90Y


PretreatmentPretreatment

Ashing the sampleg p

Adding the carrierAdding the carrier

Dissolve Sr in the sample by HNO3

Filtration


Separation of Sr from Ca by Nitrate PrecipitationSeparation of Sr from Ca by Nitrate Precipitation

Carbonate Precipitationp

Oxalate PrecipitationOxalate Precipitation

Strontium Nitrate Precipitation

Barium Chromate Precipitation


Scavenging to Separate Sr from existing YScavenging to Separate Sr from existing Y

Adding iron carrier (Fe3+) and NH4Clg ( ) 4

Adding NH OHAdding NH4OH

Filtration

Filtrate


Determination of Chemical Recovery for SrDetermination of Chemical Recovery for Sr

Precipitation in strontium carbonate p

Filtration Washing Drying the precipitateFiltration, Washing, Drying the precipitate

Weighing the Precipitate

Dissolve by HClAdd the carrier solution (Fe3+, Y3+)Store for 2 weeks


Milking of 90YMilking of Y

iron hydroxide precipitation

Filtration Acidify,

Dissolution by HClPrecipitate next milking

Filtration

Precipitate

ReviewReview

– Jelaskan Prinsip AAN dan Aplikasinya;– Jelaskan Prinsip TPI dan Aplikasinya;Jelaskan Prinsip TPI dan Aplikasinya; – Jelaskan Prinsip Titrasi Radiometri;– Jelaskan Prinsip Nuclear Dating;Jelaskan Prinsip Nuclear Dating;– Jelaskan Preparasi Radiokimia dalam Analisis

Sampel LingkunganSampel Lingkungan

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