- Email: [email protected]
Nuclear safeguards analysis: Nondestructive and analytical chemical techniques
BOOK
REVIEWS
Nuclear Safeguards Analysis: Nondestructive and Analytical Chemical niques. Edited by E. A. HAKKIIA. American Chemical Society, Washington, 1978. x + 212 pp.. $22.00.
437 TechD.C.,
This volume, the AC.5 Symposium Series 79, collects and compiles some I2 papers presented at a Symposium which was sponsored by the Division of Nuclear Chemistry and Technology, and held at the 175th Meeting of the ACS, Anaheim, California. March 13- 17. 1978. The Symposium was organized purposely to review some of the nondestructive and analytical chemical (NDA) techniques in nuclear safeguard measurement methodology including a National Standards Program. The overall safeguard program in the national laboratories is directed from the Department of Energy, Office of Safeguards and Security (DOE-OSS). It is interesting to note that nuclear safeguards have become an important factor in the public’s acceptance of nuclear energy as a source of power in the last few decades. Effective safeguarding of nuclear materials, especially high-purity plutonium (Pu) and enriched uranium (U), depends on a combination of material control and accountability and physical security. However, without the suitable measurement techniques the material control and accountability system cannot be considered adequate or sufficient because measurement provides rapid, efficient, precise. and accurate means of determining the location and quantity of strategic nuclear materials (SNM). The first paper contributed by G. Hammond and C. Auerbach of DOE-OSS considers the realm of measurements while the following two chapters by C. D. Bingham and W. P. Reed and H. T. Yolken review the standard reference materials programs operated by the New Brunswick Laboratory and the NBS. The in-line or at-line measurement techniques which rely heavily on NDA, including X-ray, y-ray, or a-particle emission or absorption, active or passive neutron interrogation, or calorimetry for standards ?:‘“U. s:‘xU. and ?:jhPuare particularly concerned in these chapters. In chap. 4, J. P. Shipley discusses the development of data evaluation methodology for diversion detection in dynamic accounting. This is a kind of decision analysis for safeguard systems. Another matematical treatment considering the nonlinear curve-fitting techniques that include both the mass uncertainty of standards and the system measurements errors are presented in Chapter 5 by W. L. Pickles, J. W. McClure. and R. H. Howell. The correlation of the key input-accountability measurements for nuclear fuel reprocessing plants with plant output measurements and with reactor operating data is illustrated in Chap. 6 by L. Koch and in Chap. 7 by C. L. Timmerman. The automatic X-ray fluorescence spectrometry. automatic isotope dilution analysis, isotope correlation techniques, and isotope safeguard techniques were briefly demonstrated with the aids of typical data that have been obtained. Chapter 8 by T. R. Canada (‘1 trl. reviews the theory of energy-dispersive absorption edge densitometry and describes its recent on-line applications to the measurements of special nuclear material such as U, Pu, and thorium (Th). Some possible future adaptations in the field of nuclear safeguards are also mentioned. The following chapter by K. J. Hofstetter cf cl/. also deals with the NDA instrumentation methods on applications of on-line n-monitors to process streams in a nuclear fuel reprocessing plant. The analyses of standard uranium ore. ‘,litJ, and ‘,‘“Pu samples with a well-type Ge(Li) detector are investigated and reported by F. P. Brauer et rrl. in Chap. IO. Special applications of X-ray and n-ray spectrometric measurements coupled with the multichannel analyzer microprocessor and with minicomputer system for data treatment are critically discussed. Calorimetric assay provides a precise, nondestructive method to determine Pu content in a sample based on the heat emitted by decaying radionuclides. This technique is applicable
438
BOOK
REVIEWS
to sealed containers and is essentially independent of sample matrix configuration and elemental composition. The operating characteristics of a portable calorimeter designed for assaying mixed-oxide powers, fuel pellets, and Pu-containing solutions are discussed by C. T. Roche PI ul. in Chap. I I. Finally, the cumulative successful experience of performance of a uranium accountability system at an operating fuel reprocessing facility in the Idaho Chemical Processing Plant (ICPP) for 25 years is reported by M. A. Wade et rrl. A detailed description of sampling, analytical methodology, calibration procedures traceability, and quality control with mass spectrometry is clearly provided.
Analytical Chemistry of Liquid Fuel Sources: Tar Sands, Oil Shale, Coal, and Petroleum. Edited by P. C. UDEN, S. SIGGIA, AND H. B. JENSEN. American Chemical Society, Washington, D.C., 1978. ix + 341 pp., $32.00. This volume is the Advances in Chemistry Series 170 of the American Chemical Society. It collects and compiles some 21 papers presented at a Symposium which was cosponsored by the Division of Petroleum Chemistry and Analytical Chemistry at the 173rd Meeting of the American Chemical Society, New Orleans, Louisiana, March 21-25, 1977. It presents reviews of ongoing research and development in the various areas of liquid fuel analysis and characterization, emphasizing the current advances in specific analytical methodology and instrumentation. This Symposium brings together some 70 presently active energy expertise from the diverse fields of energy resources investigation and analysis. About 320 up-to-date literature have been cited in this volume. A complete index is included. The analytical methods ranged from high-resolution gas and liquid chromatography to electron microprobe, carbon-13 NMR, EPR, and computer modeling. Great efforts were also made to indicate where techniques developed in one fuel liquids area could be applied usefully in others. The subject materials cover generally the examination of structural characterization of solvent-refined coals; the chemistry and composition of petroleum asphaltenes; chromatographic studies on oil sand bitumens: discussion of organometallic complexes in domestic tar sands: electron microprobe studies of Green River and Devonian oil shale: the hydrotreating response of coal, shale, and petroleum liquids: and HPLC techniques for analysis of residual fractions. This volume could be considered not only an excellent reference book for the energy sources study and analysis but also an valuable guidebook for practical analytical methodology and application instrumentations. The opening chapter by W. A. Schmeling ct ml. discusses the development of a simplified test method for field lab/mine applications. Eighteen subbituminous coal samples were tested for their liability to spontaneous combustion using a combination of temperatureprogrammed air oxidation and gas-liquid chromatography (GLC). The next paper by E. J. Gallegos describes the results of a detailed analysis of five U.S. coals of differing geological history using the technique of pyrolysis GC-MS-computer and thermal gravimetry-mass spectrometry-computer (TG-MS-C). It demonstrates the fantastic power of the combination of these techniques for analysis of complex nonvolatile coal systems to obtain both qualitative and quantitative information. A quantitative ‘H and l”C NMR study of the organic constituents in different solventrefined coals (SRC) as a function of the feed coal is reported by D. L. Wooton rt trl. in Chap. 3. Chapter 4 also reviews the analysis of SRC. recycle solvents, and coal liquefaction products with column chromatography of GC-MS techniques by J. E. Schiller. The
REVIEWS
Nuclear Safeguards Analysis: Nondestructive and Analytical Chemical niques. Edited by E. A. HAKKIIA. American Chemical Society, Washington, 1978. x + 212 pp.. $22.00.
437 TechD.C.,
This volume, the AC.5 Symposium Series 79, collects and compiles some I2 papers presented at a Symposium which was sponsored by the Division of Nuclear Chemistry and Technology, and held at the 175th Meeting of the ACS, Anaheim, California. March 13- 17. 1978. The Symposium was organized purposely to review some of the nondestructive and analytical chemical (NDA) techniques in nuclear safeguard measurement methodology including a National Standards Program. The overall safeguard program in the national laboratories is directed from the Department of Energy, Office of Safeguards and Security (DOE-OSS). It is interesting to note that nuclear safeguards have become an important factor in the public’s acceptance of nuclear energy as a source of power in the last few decades. Effective safeguarding of nuclear materials, especially high-purity plutonium (Pu) and enriched uranium (U), depends on a combination of material control and accountability and physical security. However, without the suitable measurement techniques the material control and accountability system cannot be considered adequate or sufficient because measurement provides rapid, efficient, precise. and accurate means of determining the location and quantity of strategic nuclear materials (SNM). The first paper contributed by G. Hammond and C. Auerbach of DOE-OSS considers the realm of measurements while the following two chapters by C. D. Bingham and W. P. Reed and H. T. Yolken review the standard reference materials programs operated by the New Brunswick Laboratory and the NBS. The in-line or at-line measurement techniques which rely heavily on NDA, including X-ray, y-ray, or a-particle emission or absorption, active or passive neutron interrogation, or calorimetry for standards ?:‘“U. s:‘xU. and ?:jhPuare particularly concerned in these chapters. In chap. 4, J. P. Shipley discusses the development of data evaluation methodology for diversion detection in dynamic accounting. This is a kind of decision analysis for safeguard systems. Another matematical treatment considering the nonlinear curve-fitting techniques that include both the mass uncertainty of standards and the system measurements errors are presented in Chapter 5 by W. L. Pickles, J. W. McClure. and R. H. Howell. The correlation of the key input-accountability measurements for nuclear fuel reprocessing plants with plant output measurements and with reactor operating data is illustrated in Chap. 6 by L. Koch and in Chap. 7 by C. L. Timmerman. The automatic X-ray fluorescence spectrometry. automatic isotope dilution analysis, isotope correlation techniques, and isotope safeguard techniques were briefly demonstrated with the aids of typical data that have been obtained. Chapter 8 by T. R. Canada (‘1 trl. reviews the theory of energy-dispersive absorption edge densitometry and describes its recent on-line applications to the measurements of special nuclear material such as U, Pu, and thorium (Th). Some possible future adaptations in the field of nuclear safeguards are also mentioned. The following chapter by K. J. Hofstetter cf cl/. also deals with the NDA instrumentation methods on applications of on-line n-monitors to process streams in a nuclear fuel reprocessing plant. The analyses of standard uranium ore. ‘,litJ, and ‘,‘“Pu samples with a well-type Ge(Li) detector are investigated and reported by F. P. Brauer et rrl. in Chap. IO. Special applications of X-ray and n-ray spectrometric measurements coupled with the multichannel analyzer microprocessor and with minicomputer system for data treatment are critically discussed. Calorimetric assay provides a precise, nondestructive method to determine Pu content in a sample based on the heat emitted by decaying radionuclides. This technique is applicable
438
BOOK
REVIEWS
to sealed containers and is essentially independent of sample matrix configuration and elemental composition. The operating characteristics of a portable calorimeter designed for assaying mixed-oxide powers, fuel pellets, and Pu-containing solutions are discussed by C. T. Roche PI ul. in Chap. I I. Finally, the cumulative successful experience of performance of a uranium accountability system at an operating fuel reprocessing facility in the Idaho Chemical Processing Plant (ICPP) for 25 years is reported by M. A. Wade et rrl. A detailed description of sampling, analytical methodology, calibration procedures traceability, and quality control with mass spectrometry is clearly provided.
Analytical Chemistry of Liquid Fuel Sources: Tar Sands, Oil Shale, Coal, and Petroleum. Edited by P. C. UDEN, S. SIGGIA, AND H. B. JENSEN. American Chemical Society, Washington, D.C., 1978. ix + 341 pp., $32.00. This volume is the Advances in Chemistry Series 170 of the American Chemical Society. It collects and compiles some 21 papers presented at a Symposium which was cosponsored by the Division of Petroleum Chemistry and Analytical Chemistry at the 173rd Meeting of the American Chemical Society, New Orleans, Louisiana, March 21-25, 1977. It presents reviews of ongoing research and development in the various areas of liquid fuel analysis and characterization, emphasizing the current advances in specific analytical methodology and instrumentation. This Symposium brings together some 70 presently active energy expertise from the diverse fields of energy resources investigation and analysis. About 320 up-to-date literature have been cited in this volume. A complete index is included. The analytical methods ranged from high-resolution gas and liquid chromatography to electron microprobe, carbon-13 NMR, EPR, and computer modeling. Great efforts were also made to indicate where techniques developed in one fuel liquids area could be applied usefully in others. The subject materials cover generally the examination of structural characterization of solvent-refined coals; the chemistry and composition of petroleum asphaltenes; chromatographic studies on oil sand bitumens: discussion of organometallic complexes in domestic tar sands: electron microprobe studies of Green River and Devonian oil shale: the hydrotreating response of coal, shale, and petroleum liquids: and HPLC techniques for analysis of residual fractions. This volume could be considered not only an excellent reference book for the energy sources study and analysis but also an valuable guidebook for practical analytical methodology and application instrumentations. The opening chapter by W. A. Schmeling ct ml. discusses the development of a simplified test method for field lab/mine applications. Eighteen subbituminous coal samples were tested for their liability to spontaneous combustion using a combination of temperatureprogrammed air oxidation and gas-liquid chromatography (GLC). The next paper by E. J. Gallegos describes the results of a detailed analysis of five U.S. coals of differing geological history using the technique of pyrolysis GC-MS-computer and thermal gravimetry-mass spectrometry-computer (TG-MS-C). It demonstrates the fantastic power of the combination of these techniques for analysis of complex nonvolatile coal systems to obtain both qualitative and quantitative information. A quantitative ‘H and l”C NMR study of the organic constituents in different solventrefined coals (SRC) as a function of the feed coal is reported by D. L. Wooton rt trl. in Chap. 3. Chapter 4 also reviews the analysis of SRC. recycle solvents, and coal liquefaction products with column chromatography of GC-MS techniques by J. E. Schiller. The