Experimental validation of nuclear data in the k0 standardized neutron activation analysis using the dalat research reactor

MINISTRY OF EDUCATION AND MINISTRY OF SCIENCE AND TRAINING TECHNOLOGY VIETNAM ATOMIC ENERGY INSTITUTE Phonesavanh Lathdavong EXPERIMENTAL VALIDATION OF NUCLEAR DATA IN THE k0-STANDARDIZED NEUTRON ACTIVATION ANALYSIS USING THE DALAT RESEARCH REACTOR Dissertation for the Doctor Degree of Atomic and Nuclear Physics Ho Chi Minh City, Vietnam – 2023 MINISTRY OF EDUCATION AND MINISTRY OF SCIENCE AND TRAINING TECHNOLOGY VIETNAM ATOMIC ENERGY INSTITUTE Phonesavanh Lathdavong EXPERIMENTAL VALIDATION OF NUCLEAR DATA IN THE k0-STANDARDIZED NEUTRON ACTIVATION ANALYSIS USING THE DALAT RESEARCH REACTOR Majors: Atomic and nuclear physics Code: 9.44.01.06 Supervisors: Assoc Prof Dr Ho Manh Dung Dr Hoang Sy Minh Tuan Ho Chi Minh City, Vietnam – 2023 Dedication I dedicate my dissertation work to my parents, brother, and sister, as well as to my love, whose words of encouragement and constant support have been with me throughout the entire challenging years of my doctorate program Their unwavering love and care have always been beside me, and I am forever grateful for their support Ho Chi Minh City, … December 2023 Phonesavanh LATHDAVONG i Acknowledgments First of all, I would like to express my sincere gratitude to my supervisors, Assoc Prof Dr Ho Manh Dung and Dr Hoang Sy Minh Tuan, for their invaluable guidance and support throughout my studies Their practical insights and advice were instrumental in leading me through my dissertation thesis, and they provided numerous beneficial incentives for my future professional activities I would also like to thank the Nuclear Training Center, which is belonging to Vietnam Atomic Energy Institute (VINATOM) for their excellent facilitation of all arrangements and documentation Furthermore, I extend my gratitude to the Dalat Nuclear Research Reactor (DNRR) and the Center for Nuclear Technologies (CNT) in Ho Chi Minh City, particularly Dr Ho Van Doanh, for their collaboration and accommodations during my Ph.D program I am grateful to the International Atomic Energy Agency (IAEA) for their partial financial support and encouragement towards achieving my Ph.D goals I would also like to acknowledge the generosity of my committee members for their expertise and precious time Finally, I wish to express my heartfelt thanks to my beloved parents, siblings, colleagues, and institutional fellows for nurturing and establishing a conducive environment for my education ii Contents Pages Dedication i Acknowledgments ii Content iii List of Symbols vii Greek Alphabet ix List of Abbreviations xi List of Figures xii List of Tables xiv Tóm tắt .1 Abstract .2 Introduction Chapter The Overview of Neutron Activation Analysis .5 1.1 General Information 1.2 Neutron activation analysis as a trace element analytical method .6 1.2.1 Advantages of Neutron Activation Analysis 1.2.2 Disadvantages of Neutron Activation Analysis 1.3 Applications 10 1.3.1 Biology 10 1.3.2 Environment 10 1.3.3 Industry 11 1.3.4 Geology 11 iii 1.3.5 Archaeology 11 1.4 Neutron Flux 12 1.4.1 Thermal neutrons 13 1.4.2 Epithermal neutrons 14 1.4.3 Fast neutron 15 1.5 Introduction to k0-NAA 15 1.6 Introduction to Q0 factor 17 1.7 Determination of k0,Au factors 18 1.8 Determination of Q0 factors 18 1.9 Determination of α, ƒ, 𝜙th 19 1.10 QA and QC for k0-NAA 20 1.11 The reference materials .20 1.12 The reason to conduct the experiment of this dissertation 23 1.13 Purpose of the dissertation 23 1.14 Dissertation outline 25 Chapter Theoretical methods of neutron activation analysis .26 2.1 Theoretical aspects of neutron activation analysis 26 2.1.1 Types of neutron activation analysis 26 2.1.2 Selective Activation 30 2.1.3 Derivation of computational equations .30 2.1.3.1 Activation 30 2.1.3.2 Radioactive decay .31 2.1.3.3 Measurement .34 2.1.3.4 Detection limit 35 iv 2.2 Standardization methods of neutron activation analysis 37 2.2.1 Absolute standardization method 37 2.2.2 Relative standardization method .39 2.2.3 Single-comparator standardization method 42 2.2.4 The k0 standardization method 43 2.2.1 The k0-NAA in different approaches 44 2.2.2 The k0 factor for complex decay .44 2.2.3 The k0 factors for threshold reactions .44 2.2.4 The k0 and Westcott formalization 45 2.3 The implementation of k0-standardization on DNRR .46 2.3.1 Calibration of HPGe detector 46 2.3.2 Full-energy peak detection efficiency .46 2.3.3 Peak-to-total ratio calibration 48 2.3.4 FWHM calibration 50 2.4 Neutron spectrum parameter determination .50 2.4.1 Determination of α 50 2.4.2 Determination of ƒ 52 2.4.3 Comparator Fc and thermal neutron fluence rate determination 52 2.5 Validation of method 53 2.5.1 Precision 53 2.5.2 Accuracy 54 2.5.3 Linearity 54 2.5.4 Detection limit 54 2.5.5 Robustness 55 v 2.5.6 Selectivity 55 2.5.7 Traceability .56 2.6 Calculations .56 2.6.1 Determinaiton of k0 factors .56 2.6.2 Determinaiton of Q0 factors 58 Chapter Experimental in Dalat nuclear research reactor .58 3.1 Designation of the DNRR 58 3.2 Introduction to Irradiation system for k0-NAA on DNRR 61 3.2.1 The Channel 7-1 as sample irradiation system in the DNRR 62 3.2.2 The k0-NAA in Dalat nuclear research reactor 64 3.3 Practical Experiment in Dalat nuclear research reactor 65 3.2.1 Sample preparation 65 3.2.2 Prepare monitors .68 3.2.3 Measurement of monitors 69 3.2.4 The use of specialized program k0-IAEA 69 3.2.5 Sample irradiation of the seven short-lived radionuclides 70 3.2.6 Calibration of neutron spectra in Channel 7-1 71 3.2.7 Irradiation measurement 72 Chapter Results and discussion 73 4.1 Results .73 4.2 Discussions .74 4.2.1 Research results 74 4.3 Conclusions and future work 86 4.3.1 Conclusions 86 vi 4.3.2 New points of discussion 87 4.3.3 Future plan 88 Papers published using for the dissertation 89 References 90 vii List of Symbols Symbols Meaning A Activity Asp Specific activity A0 Activity created at the end of irradiation C Correction for decay during counting c Concentration COI Correction factor for true-coincidence effects E Neutron energy E0 (Maxwellian) neutron energy (0.025 eV) ECd Effective Cd cut-off energy (0.55 eV in mm Cd) Er Effective resonance energy f Thermal to epithermal neutron flux ratio fF Ratio of thermal neutron flux to fast neutron flux Gth Correction factor for thermal neutron self-shielding Ge Correction factor for epithermal neutron self-shielding I0 Resonance integral M Mass number NA Avogadro number Np Number of counts in full-energy peak corrected for pulse losses N0 Number of target nuclei n(v) neutron density per unit of velocity at neutron velocity v Q0 Resonance integral (1/E) to 2200 m·s-1 cross-section ratio Q0(α) Resonance integral (1/E1+α) to 2200 m·s-1 cross-section ratio R Reaction rate per nucleus capturing a neutron RCd Cadmium ratio viii 140 La are in good agreement with the recommended reference values [16, 26, 41, 42] There is no true coincident effect, and the accuracy of the efficiency transfer computations is high The differences between this work and the reference ones are typically 3-5%, sometimes higher for the lowest-yield lines The k0 results shown in Table 4.3 significantly differ from the reference [10] at a 95% confidence level There were two energy ranges for the 56Mn experiment: 846.8 keV and 1810.7 keV The results are shown in Fig 4.11 and 4.12, with values of 4.89×10-1 and 1.31×10-1, respectively The experimental results for 56Mn with two energy ranges of 846.8 keV and 1810.7 keV are shown in Fig 4.11 and Fig 4.12, with values of 4.89×10-1 and 1.31×10-1, respectively The experimental values are in good agreement with the recommended references [16, 26, 41, 42] The k0 factors obtained for 56Mn are listed in Table 4.1, and there is no significant difference between the determined and assigned values Additionally, there is no coincidence effect, and these values are within acceptable limits for short irradiation, quick transfer, and quick counting Page 83 of 97 Table 4.4 The comparison of analysis results (mg/kg) based on the experimented and referenced k0,Au factors Ce Radionuclides Elements Ue Using k0,Au factors (experiment) Cr Ur Using k0,Au factors (reference) Cc Uc Certified values Ce / Cc Cr / Cc Experiment/ Certified Reference/ Certified V 52V 38 42 39 0.97 1.08 Cu 66Cu 4284 171 4039 3930 118 1.09 1.03 Cl 38Cl 4407 176 4313 173 4330 173 1.02 1.00 Cs 134mCs 934 56 776 47 897 36 1.04 0.87 I 128I 151 143 152 0.99 0.94 La 140La 267 19 254 18 265 11 1.01 0.96 Mn 56Mn 111 108 114 0.97 0.95 Remarks: Ce and Ue - The experimental concentrations and uncertainties, respectively obtained using the k0,Au values in this work; Cr and Ue - The reference concentrations and uncertainties, respectively obtained using the k0,Au values from references of DeCort, 2003 [17]; Cc and Uc - The certified concentrations and uncertainties of the certified reference material (SMELS Type-I) The comparison of the determined k0,Au factors (Ce) experimentally with those from references (Cr) showed a good agreement with certified values (Cc) for various elements (see Table 4.4) The ratios Ce/Cc and Cr/Cc, which measure agreement, are consistently close to one, confirming that both the experimentally determined and reference k0,Au factors are reliable for analysis of the elemental concentrations of interest We carefully considered uncertainty, represented by Ue and Ur for the experimental and reference k0,Au factors resulted in a high accuracy of the k0-based method as demonstrated in this study However, upon closer investigation, there are slight differences, especially for Cu (this work) and Cs (reference) In these cases, Page 84 of 97 experimentally determined and reference values deviated from certified values of 9% and 13%, respectively This observation suggests a further research to the specific conditions or factors affecting the determination of k0,Au factors for these elements This detailed investigation would be crucial for improving the method and ensuring higher accuracy for analyses in the future In summary, Table 4.4 revealed that the dataset consists of seven elements of radionuclides were determined for the concentrations and uncertainties of the experimental and reference of k0,Au factors The value of k0,Au factors obtained in this work for some short and medium-lived radionuclides (52V, 66Cu, 38Cl, 134mCs, 128I, 140 La, and 56 Mn) have been assessed by analyzing the SMELS Type-I The deviation of the results of analysis for SMELS Type-I with the experiment and reference k0,Au factors as compared with the certified values were within ± 9.0% and ± 13.0%, respectively The comparative results showed that the experiment k0,Au factors done by this study were acceptable and better agreement as compared with the reference ones Page 85 of 97 4.3 Conclusions and future work 4.3.1 Conclusions The Dalat Nuclear Research Reactor (DNRR) was used to test and confirm the k0 factors needed for the k0-standardized neutron activation analysis (k0-NAA) Experimental validation of the k0 factors required by the k0-standardized neutron activation analysis (k0-NAA) using the Dalat Nuclear Research Reactor (DNRR) was done The new k0 factors of short and medium-lived radionuclides, were evaluated, including: 66 Cu, 52 V, 38 Cl, 134m Cs, 128 I, 140 La, and 56 Mn, which were determined at DNRR Perform the k0-NAA using the new k0 dataset to determine the concentrations of the elements in the reference materials (RMs) against the certified concentration values The difference between the experimental results of determining the new k0 factors and the reference values (literature) is less than 7% From there, applying the new k0 factors to k0-NAA at DNRR resulted in the elemental concentrations in the RMs compared to the certified values in the range of 7-11% Exception for 134m Cs, which were biased by 19% This work conducted the experiments at DNRR, including the characterization of the Channel 7-1; calibration of the gamma-ray spectrometer using the HPGe detector; and the data processing that is required by the k0-NAA method with experimental parameters (neutron field parameters, detector efficiency, corrections, etc.) The "self-characterization" method for Channel 7-1 using synthetic multi-element standard samples (SMELS I) was the first use regarded as simple and convenient experimentally, with results consistent with the conventional method using independent monitors To sum up the result of the experimental validation of nuclear data in k0-NAA as using the Dalat nuclear research reactor (DNRR) [77], it can be seen that Table 12 presents the experimentally determined k0 factor of 11 gamma-rays from radionuclides of both short- and medium-lived nuclides using the DNRR The results are compared with the recommended literature value and k0 reference It was found that the k0 factors for the short-lived radionuclides 52V at 1434.1 keV and 66Cu at 1039.2 keV, as well as the medium-lived radionuclide 128I, are similar to the k0 factors for short-lived radionuclides 66 52 V at the energy of 1434.1 keV and Cu at the energy of 1039.2 keV, as well as medium-lived radionuclides 128 I, are Page 86 of 97 determined and are in good agreement with the result of the k0 reference It is important to note that 52V, 66Cu, and 128I emit only a single gamma ray, and there is no true coincidence effect The ratio of the experiment to reference is 1.004 for both isotopes For the medium-lived radionuclides, 38Cl and 56Mn, which emit two gammarays with a high emission probability, the experimental results for determining the k0 factor are also in good agreement with the k0 reference The differences between the experiment and reference values are less than 3% For other radionuclides, such as 140 La, which had three different gamma-ray energies, the k0 factor was generally in good agreement compared to the reference information However, for 134m Cs, a medium-lived radionuclide with an energy of 127.5 keV, the experiment value was compared to the k0 reference, and the Exp./Ref ratio was 8.31E-01 The k0 factor of 134mCs has a high difference with the k0 reference value because this energy is in a low energy region (< 200 keV), and some effects from Compton or low X-ray may influence the results Thus, 134mCs appear to be not good due to low uncertainty The determination of the k0 factor measured the absolute uncertainty and was calculated based on the component of parameter error propagation The uncertainties obtained uncertainties for determining the k0 factor for short- and medium-lived radionuclides were reported in the study 4.3.2 New points of discussion To validate the k0 experiment used in my own experiments, I compare them with those reported by different authors in the field [16, 26, 41, 42] This will involve a thorough review of the literature, looking for studies that have used similar reactor and neutron spectra to those used in my experiments This comparison will be critical for validating the nuclear data used in my experiments, as well as for ensuring that my experimental results are in good agreement with the reference values Any discrepancies or differences between my k0 values and those reported in the literature will need to be carefully investigated, to ensure that my results are as accurate as possible Page 87 of 97 In addition to comparing my k0 experiment with those reported in the literature, I will also need to consider any potential sources of error in my own experiments This may involve a careful analysis of the data, looking for any systematic errors or biases that could affect the accuracy of my results I will also need to consider the effects of any uncertainties in the nuclear data used in my experiments, and to quantify these uncertainties wherever possible 4.3.2 Future plan A Future plan in this research area is proposed to investigate and re-determine the k0 factors of very short-lived radionuclides (less than 20 seconds), such as 77mSe and 20F as follows: (1) There is a lack of experimental data for these radionuclides, and additional experiments are needed to improve their accuracy and reduce the uncertainty of their k0 values (2) Re-determination of k0 factors for radionuclides with high uncertainties, such as 133Ba is needed This will help to improve the accuracy of k0 factor and increase the reliability of the k0-NAA method for the element (3) Determination of the k0 factor for 152Eu at low energy (46 keV) is proposed because it is missing in the current k0 dataset By addressing the future plan as outlined above, some works are necessary to further perform, thereby improving the accuracy and reliability of the k0-NAA for radionuclides of interest can be improved It is aiming at developing the method to be applied to a wider range of radionuclides with different energies Page 88 of 97 Papers published using for the dissertation Ho Manh Dung, Tran Tuan Anh, Tran Quang Thien, Ho Van Doanh, Truong Truong Son, Phonesavanh Lathdavong, Analysis of automobile window glass samples by the k0-based Neutron Activation Analysis for forensic applications, Journal of Radioanalytical and Nuclear Chemistry, Volume 332 (2023) 34933498; Ho Manh Dung, Phonesavanh Lathdavong, A review of nuclear data for the k0based neutron activation analysis, Journal of Nuclear Science and Technology, Vietnam, Vol.9, No (2019) 28-33; Phonesavanh Lathdavong, Ho Manh Dung, Tran Quang Thien, Doanh Van Ho, Son Truong Truong, Self-characterization of irradiation facility using synthetic multi-element standard (SMELS) for the determination of k0-factors of seven radionuclides of interest, Journal of Nuclear Science and Technology, Vietnam, accepted for publishing in September 2023; Ho Manh Dung, Tran Tuan Anh, Ho Van Doanh, Tran Quang Thien, Nguyen Thi Tho, Trinh Van Cuong, Truong Truong Son, Phonesavanh Lathdavong, Evaluation of “k0-DALAT” software for the k0-Standardized neutron activation analysis, VINANST-14, Da Lat, 09-10/12/2021 Page 89 of 97 References [1] Gibbons, 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