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Title Page

ABSTRACT

Contents

I. Introduction 12

II. What is Nuclear Forensics? 13

III. Literature Review: LIBS 18

3.1. LIBS Principles 18

3.2. Reduction of Instrument Size 22

3.3. Remote Detection and Analysis 26

3.4. Analysis in Liquid Matrix 33

3.5. Isotopes Analysis 35

3.6. New Isotopes Analysis Technique: LAMIS 39

IV. Material Selection: Theft Scenarios of Radioactive Materials 45

4.1. Pathway Analysis until Disposal 46

4.2. Historical Cases: Theft Attempts and Incidents 48

4.3. Evaluation of Theft Possibility from Nuclear Facilities and Devices 49

4.3.1. Reprocessing and Interim Storage Facility 49

4.3.2. Dismantling and Production Facility 58

4.3.3. Industrial Devices 60

4.4. Material Selection 61

V. Experiment: Post-Detonation of RDDs 63

5.1. Experimental Methods 63

5.1.1. Samples Preparation 63

5.1.2. Analytical Tools 65

5.2. Results and Discussion 67

5.2.1. Experiment 1: Reference Samples Analysis 67

5.2.2. Experiment 2: Simulated Samples Analysis 79

5.2.3. Suggestion of On-Site Analysis Algorithm for Nuclear Forensics 86

VI. Conclusion 88

REFERENCES 89

List of Tables

Table 1. Recommended categories for nuclear materials. 14

Table 2. Recommended categories for radioactive sources used in common practices. 15

Table 3. Examples of relevant radionuclide signatures. 16

Table 4. Nuclear forensic activities following a terrorist explosion. 16

Table 5. Comparison of on-site NDA techniques. 17

Table 6. LIBS groups that started in the period 1975 to 2000. 21

Table 7. LIBS LODs of radioactive surrogates when encountered on surfaces of different common urban materials. 32

Table 8. Molecular isotope shifts calculated using molecular constants. 40

Table 9. Basic radiological properties of 9 key radionuclides for RDDs. 45

Table 10. Sr fuel compounds. 47

Table 11. Location of RTG theft attempts and incidents in Soviet and Russia. 48

Table 12. Comparative analysis of various security regulations of nuclear materials. 50

Table 13. INFCIRC/225 categorization of nuclear material. 51

Table 14. Proposed categorization of U-235-containing material to U.S. NRC. 51

Table 15. Proposed categorization of Pu/U-233-containing material to U.S. NRC. 52

Table 16. U.S. DOE attractiveness levels of nuclear material. 52

Table 17. U.S. DOE nuclear material categorization [graded safeguards table]. 53

Table 18. Bunn's nuclear material categorization proposed in 2014. 54

Table 19. Bunn's attractiveness levels and discount factors proposed in 2014. 54

Table 20. FOM mapped to U.S. DOE attractiveness level. 55

Table 21. Mass of target item after 10 years of cooling. 56

Table 22. Attractiveness level results when applied to pyroprocessing. 57

Table 23. Categorization results when applied to pyroprocessing. 57

Table 24. Summary of security group performance objectives. 58

Table 25. Calculated ratio Ti:Sr of highest intensity near target wavelengths where Gaussian fitting... 74

Table 26. Calculated SNRs and LODs (± 95% confidence interval) for simulated samples at target wavelengths of 460.7㎚ and 707.0㎚. 83

List of Figures

Figure 1. The nuclear forensics process. 13

Figure 2. Comparison of techniques for nuclear forensics. 17

Figure 3. Schematic diagram of LIBS. 18

Figure 4. Schematic diagram of LIBS system. 19

Figure 5. Prototype Be monitor based on LIBS. 22

Figure 6. The portable LIBS surface analyzer. 23

Figure 7. Schematic diagram of the TRACER instrument. 23

Figure 8. Russian built LIBS instrument. 24

Figure 9. Portable LIBS system of CNSC. 24

Figure 10. LIBS test sample of yellow cake normalized class membership probability against three... 25

Figure 11. Layout of the LIBS instrument on the K9 rover. 26

Figure 12. Examples of LIBS detection system designs developed by Applied Photonics Ltd. 27

Figure 13. Schematic diagram of Teramobile LIBS system. 28

Figure 14. Schematic diagram of standoff LIBS apparatus. 28

Figure 15. Standoff LIBS spectra of the tested blank supports. 30

Figure 16. Standoff LIBS spectra for different residues of radioactive surrogates on aluminum. 30

Figure 17. The diver working at a 30 meter depth. 33

Figure 18. Calibration curves for Fe I 387.857㎚ line (top) and Na I 330.2㎚ doublet line (bottom). 34

Figure 19. Spectrum of enriched uranium (93.5% 235U, 5.3% 238U) obtained with a single-channel...(이미지참조) 35

Figure 20. LIBS spectrum of plutonium metal sample with isotope ratio 93/6. 36

Figure 21. LIBS spectrum of plutonium oxide sample with isotope ratio 49/51. 36

Figure 22. (a) Person-portable LIBS backpack instrument. (b) P1C probe used here showing sampling... 38

Figure 23. Molecular vs. atomic isotopic shifts for various elements, taken from Stern and... 39

Figure 24. The emission spectra from ablation of the SrCO3 sample at different delay times on a semi-... 41

Figure 25. Simulated emission spectra of the (2,0) band of the A→X system for 90SrO, 88SrO, 87SrO,...(이미지참조) 42

Figure 26. Experimental emission spectra of the (2,0) band of the A→X system of SrO measured from... 42

Figure 27. Spectra of diatomic molecules obtained from ablation of SrCO₃, SrF₂, SrCl₂, SrBr₂, and... 43

Figure 28. SrF2 waste capsule. 46

Figure 29. Beta-M type RTG. 47

Figure 30. Five target components of the pyroprocessing analysis. 56

Figure 31. Steps in processing of 90Sr fuel.(이미지참조) 59

Figure 32. Retired RTGs on the Kola Peninsula. Photo courtesy of Bellona. 60

Figure 33. Theft scenarios of 90Sr radioactive materials.(이미지참조) 62

Figure 34. Experiment at the Sandia National Laboratories showing a dispersal pattern of the... 63

Figure 35. Photo of simulated samples. 64

Figure 36. Flow chart of experiment. 66

Figure 37. SEM image of blank Al substrate. 67

Figure 38. SEM/EDX result of blank mortar substrate. 68

Figure 39. SEM/EDX result of blank soil substrate. 68

Figure 40. SEM image of SrCO₃ powder. 69

Figure 41. SEM image of SrF₂ powder. 69

Figure 42. SEM image of SrTiO₃ powder. 69

Figure 43. Spectrum of blank Al substrate. 70

Figure 44. Characteristic wavelengths (308.2, 309.2, 394.4, and 396.2 ㎚) of blank Al substrate. 70

Figure 45. Spectrum of blank mortar substrate compared with that of Gaona et al. 71

Figure 46. Characteristic wavelengths (393.4 and 396.8 ㎚) of blank mortar substrate. 71

Figure 47. Spectrum of blank soil substrate compared with that of Al. 72

Figure 48. Characteristic Na (589.0, 589.6 ㎚) and K (766.5, 769.9 ㎚) peaks of blank soil substrate. 72

Figure 49. Example of LIBS spectra and characteristic peaks of Zr. 73

Figure 50. Gaussian fitting of Ti peaks of SrTiO₃. 73

Figure 51. Comparison of SrF₂ and SrCO₃ spectra in SrF radical band (577-588 ㎚) region. 74

Figure 52. Integration of region in 577-585㎚. The area was calibrated by assuming that Sr peak at... 75

Figure 53. Raman spectrum of SrCO₃. 76

Figure 54. Raman spectrum of SrF₂. 76

Figure 55. Raman spectrum of SrTiO₃. 77

Figure 56. Raman spectrum of blank Al substrate. 77

Figure 57. Raman spectrum of blank mortar substrate. 78

Figure 58. Schematic diagram of experiment 2. 79

Figure 59. Example of LIBS spectra of simulated samples: materials on Al substrate. 79

Figure 60. Comparison of quantified ratio Ti:Sr at Sr target wavelength of 460.7㎚. 80

Figure 61. Comparison of quantified ratio Ti:Sr at Sr target wavelength of 707.0㎚. 80

Figure 62. Comparison of RSDs for each substrate. 81

Figure 63. Box plot of blank substrate intensities at 460.7㎚. 82

Figure 64. Box plot of blank substrate intensities at 707.0㎚. 82

Figure 65. SEM images of Al substrate after laser shot. 84

Figure 66. SEM images of mortar substrate after laser shot. 84

Figure 67. SEM images of soil substrate after laser shot. 84

Figure 68. 1994 Munich Pu mixture (weapon-grade Pu + high-burn-up fuel). 85

Figure 69. The principle of simultaneous acquisition of LIBS and Raman information using a single... 86

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