Aplikasi Teknik Nuklir Bid Bidang Ki Kimia i
Pusat Pendidikan dan Pelatihan Badan Tenaga Nuklir Nasional
Latar Belakang g • Perkembangan Teknologi Nuklir : • Industri • Kedokteran • Lingkungan
• Dukungan D k bid bidang R Radiokimia di ki i
Tujuan Peserta bisa menjelaskan Aplikasi Teknik Nuklir d l dalam Bid Bidang Ki Kimia i Khusus : – Menjelaskan prinsip AAN – Menjelaskan prinsip Teknik Pengenceran Isotop – Menjelaskan prinsip Titrasi Radiometri – Menjelaskan prinsip nuclear dating – Menjelaskan aplikasi untuk analisis radioaktivitas lingkungan
Sistematika • Bab I • Bab II
• Bab III • Bab IV
: Pendahuluan : Analisis Unsur 1. Analisis Aktivasi Neutron 2. Teknik Pengenceran Isotop 3. Titrasi Radiometri : Nuclear Dating : Analisis Radioaktivitas LIngkungan
Bab II Analisis Unsur
Prinsip AAN
Formulasi Aktivasi R = . .N
A N 1 e
tir
mN Av t ir A 1 e M
Proses Aktivasi dan Peluruhan
Tampang Lintang T Tangkapan k Neutron N t Thermal Th l (n,)
Target
(n,)
23Na
0,4
63Cu
4.5
26Mg
0.038
75As
4.3
27Al
0.23
81Br
2.4
37Cl
0.43
109Ag
91
48Ca
1 09 1.09
139La
89 8.9
51V
4.9
152Sm
206
50Cr
15.9
151Eu
9200
55Mn
13.3
186W
37.9
58Fe
1.28
191Ir
954
59Co
37.2
197Au
98.7
Target
Metode AAN
• • • •
Metode Absolut Metode Komparator Tunggal Metode Relatif Metode ko
Spektrum Gamma
Sensitivitas / Limit Deteksi Sensitivitas picograms g 1
1 - 10
Elements
Dy, Eu 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 - 1E4
Al, Ba, Cd, Ce, Cr, Hg, Kr, Gd, Ge, Mo, Na, Nd, Ni, Os, Pd, Rb, Rh Ru, Rh, Ru Sr, Sr Te, Te Zn, Zn Zr
1E4 - 1E5
Bi, Ca, K, Mg, P, Pt, Si, Sn, Ti, Tl, Xe, Y
1E5 - 1E6
F, Fe, Nb, Ne
1E7
Pb, S
Aplikasi AAN • Lingkungan : – Analsis Pencemaran logam berat – Pemetaan Geokimia
• Kesehatan K h t : – Analisis logam berat dalam makanan dan jaringan – Penelitian P liti d dalam l pengembangan b pengobatan b t penyakit kit
• Pangan : kandungan unsur mikro dalam bahan makanan • Industri : – kualitas batu bara, – batuan dalam sumur
Teknik Pengenceran Isotop (TPI) • pekat
encer pengenceran
•
S' m m ' 1 S
Radioisotop : memancarkan radiasi, mudah diukur
m = massa/volume zat radioaktif m’ m = massa/volume bahan yang dianalisis S’ = aktivitas jenis zat radioaktif pengenceran g S = aktivitas jjenis setelah p
Aplikasi TPI • Pengukuran Volume fluida di dalam tanah • Kedokteran Nuklir • Analisis A li i K Kuantitatif tit tif U Unsur
Titrasi Radiometri • Merupakan analisis kuantitatif • Seperti titrasi biasa, biasa tetapi senyawa hasil mudah dipisahkan • Titik akhir titrasi ditunjukkan oleh perubahan aktivitas secara mencolok
Volume
Volume
Bab III Nuclear Dating
Prinsip Nuclear Dating •Umur batuan : 238U/206Pb •Tidak mengandung uranium : 40K/40Ar 40
40
K + -11e Ar
9
(t1/2 =13 1,3 . 10 tahun tahun))
Material yang berasal dari makhluk hidup : 14C/12C
Preparasi Radiokimia untuk Analisis Radioaktivitas Lingkungan 1. Analisis137Cs dalam Sampel Air Laut 2. Analisis 222Rn dalam Sampel p Air 3. Analsis U dan Pu dalam Sampel Tanah 4. Analisis 90Sr dalam Sampel Lingkungan
Radiochemical Preparation for Analysis of 137Cs in Seawater • Average Activity 2 Bq/m3 • Sample volume : 20 L • Radioactivity Measurement by Gamma Spectrometer
• The purpose of preparation : • to collect Cs from a large sample size • to avoid self-absorption self absorption • to make easier in radioactivity measurement
Radiochemical Preparation for Analysis of 137Cs in Seawater Seawater 5 L Add 100 mL of 3 M HCl for washing the container Add Cs carrier, 2 gr AMP Stir for 30 minutes St d more than Stand th 12 h hours Decantation Filter
precipitate* precipitate
supernatant liquid** liquid
Radiochemical Preparation y of 137Cs in Seawater for Analysis precipitate* precipitate Add 2 M HCl (for washing) precipitate (MnO2) mix G Gamma Spectrometry S t t
supernatant p liquid** q Adjust pH 8.0-8.5 with NH4OH Add 10 g MnO2 powder Stir for 30 minutes Stand for more 12 hours Decantation Filter
precipitate mix
supernatant
Preparasi Radiokimia untuk t k Analisis A li i 222Rn R d dalam l S Sampell Ai Air S Sampel l air i + xylene y Ekstraksi
Fasa organik + Sintilator Pengukuran dengan LSC
Radiochemical Preparation for Analysis of Actinides ( U and Pu) in Soil U
Pu
Activity Level 0.2 mg/Kg
40 mBq/Kg
S Sample l mass 10 g
50 g
• Radioactivity Measurement by Alpha Spectrometer • The Th purpose off preparation ti : • to avoid self-absorption • to separate other radionuclides
Radiochemical Preparation for Analysis of Pu in Soil
Pretreatment
Solvent Extraction
Ion Exchange
Preparation for Electrodeposition
Electrodeposition
Radiochemical Preparation for Analysis of Pu in Soil P t t Pretreatment t
Soil Heat at 105oC for 2 hours Heat at 500oC for 4 hours Add 242Pu standard solution Add 8 M HNO3 Filter
Residue
Filtrate
Radiochemical Preparation for Analysis of Pu in Soil Purification by Solvent Extraction
Filtrate Add TOA-xylene Extract Add 8 M HNO3 Extract Add 10 M HCl Extract Add NH4I.HCl Extract
aq
org org
org aq
org aq
org
aq
Add Xylene Extract aq
Radiochemical Preparation for Analysis of Pu in Soil Purification by Solvent Extraction
Filtrate Add TOA-xylene Extract Add 8 M HNO3 Extract Add 10 M HCl Extract Add NH4I.HCl Extract
aq
org org
org aq
org aq
org
aq
Add Xylene Extract aq
Radiochemical Preparation for Analysis of Pu in Soil Purification by Ion Exchange 8 M HNO3
Filtrate
10 M HCl C NH4I.HCl
Anion Colum Dowex 1-X8, 100-200 100 200 mesh
Eluent
Radiochemical Preparation for Analysis of Pu in Soil Preparation for Electrodeposition Eluent (NH4I.HCl) Heat to dry
residue Dissolve by 2 M H2SO4 Add methylred h l d
solution (red) Add NH4OH until pH 4
solution (yellow) Add 2 M H2SO4 until p pH 2
solution (red)
Radiochemical Preparation for Analysis of Pu in Soil Electrodeposition solution (red) Pt anode
0.5 Ampere, 2 hours Add NH4OH
Stainless steel cathode
Radiochemical Preparation for Analysis of Pu in Soil
Radiochemical Preparation for Analysis of 90Sr • Radioactivity Measurement through 90Y by β Counter (Low Backgroud Counter)
• The purpose of preparation : • To separate from other radionuclides • to t isolate i l t 90Y
Radiochemical Preparation for Analysis of 90Sr 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
Radiochemical Preparation for Analysis of 90Sr Pretreatment Ashing g the sample p
Adding the carrier
Dissolve Sr in the sample by HNO3 Filtration
Radiochemical Preparation for Analysis of 90Sr Separation of Sr from Ca by Nitrate Precipitation Carbonate Precipitation p
Oxalate Precipitation
Strontium Nitrate Precipitation
Barium Chromate Precipitation
Radiochemical Preparation for Analysis of 90Sr Scavenging to Separate Sr from existing Y Adding g iron carrier ((Fe3+) and NH4Cl
Adding NH4OH Filtration
Filtrate
Radiochemical Preparation for Analysis of 90Sr Determination of Chemical Recovery for Sr Precipitation p in strontium carbonate
Filtration Washing Filtration, Washing, Drying the precipitate
Weighing the Precipitate Dissolve by HCl Add the carrier solution (Fe3+, Y3+) Store for 2 weeks
Radiochemical Preparation for Analysis of 90Sr Milking of 90Y iron hydroxide precipitation Filtration Precipitate Dissolution by HCl Filtration Precipitate
Acidify, next milking
Review – Jelaskan Prinsip AAN dan Aplikasinya; – Jelaskan Prinsip TPI dan Aplikasinya; – Jelaskan Prinsip Titrasi Radiometri; – Jelaskan Prinsip Nuclear Dating; – Jelaskan Preparasi Radiokimia dalam Analisis Sampel Lingkungan
