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Methods for Determination of Radioactive Substances in Water and Fluvial Sediments

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Methods for Determination of Radioactive Substances in Water and Fluvial Sediments i Techniques of Water-Resources Investigations of the United States Geological Survey Chapter A5 METHODS FOR DETERMINATION OF RADIOACTIVE SUBSTANCES IN WATER AND FLUVIAL SEDIMENTS By L. L. Thatcher and V. J. Janzer, U.S. Geological Survey, and K. W. Edwards, Colorado School of Mines Book 5 LABORATORY ANALYSIS UNiltED STATES DEPARTMENT OF THE INTERIOR THOlMAS S. KLEPPE, Secretary GEOLOGICAL SURVEY V. E. McKelvey, Directsr UNITED SATES GOVERNMENT PRINTING OFFICE, WASHINGTON : 1977, For sale by the Superintendent of Documents, US. Government Printing Office Washington, D.C. 20402 Stock Number 024-001-02928-6 PREFACE This series of manuals on techniques describes methods used by the Geological Survey for planning and executing water-resources investiga- tions. The material is grouped under major subject headings called books and is further subdivided into sections and chapters. Book 5 is on labora- tory analysis, Section A is on water. The unit of publication, the chapter, is limited to a narrow field of subject matter. ‘‘Metho’dsfor determination of radioactive substances in water and fluvial sediments” is the fifth chap- ter to be published under Section A of Book 5. The chapter number includes the letter of the section. The looseleaf format of this methods manual is designed to permit flexibility in revision and publication. Supplements, to be prepared as the need arises, will be issued to purchasers at no charge as they become available. 111 i i CONTENTS Page Pase Preface ______________________--__-_--_---111 Gross alpha and beta radioactivity, dissolved Abstract _______________________--___-----1 and suspended. Residue method (R-1120- Introduction _ ____ _ __ _ _ -_ -__ _ _ __ _ __ _ _ _ _ _ __ 1 76) _________________________-_________ 29 Purpose _______________________-__---1 Reference ____________________--------32 Organization _ _ _ _ _ _ -____ -- - _-_ _-- - -- -- 1 Lead-210, dissolved. Chemical separation and Nuclear data ______________________--- 2 precipitation method (R-1130-76) ------- 33 Units, symbols, and abbreviations ___--- 2 References ____________________-------37 Sources of radioactivity in water ______ 2 Radium, dissolved, as radium-226. Precipita- Natural radioactivity _____________ 2 tion method (R-1140-76) _______________ 39 Artificial radioactivity _________--- 3 Reference ____________________________ 41 Permissible concentrations of radioactiv- Radium-226, dissolved. Radon emanation ity in effluents to unrestricted areas ___ 3 method (R-1141-76) .................... 43 Radiological safety _________________-- 4 References ___________________________ 49 Geochemistry of radioactivity in water __ 4 Radium-228, dissolved. Determination by sepa- Carbon-14 ....................... 4 ration and counting of actinium-228 (R- Cesium137 and cesium-134 ________ 5 1142-76) ____________________----------51 Lead-210 ______________---------- 5 Reference ____________________________ 54 Radium ________________----------6 Radioruthenium, dissolved, as ruthenium-106. Ruthenium-106 and ruthenium-103 - 7 Distillation method (R-1150-76) 55 7 _-_-_-_-- Strontium-90 __ _ __ _ _ __ __ __ ____ __ - References __________________________ 58 Tritium (hydrogen-3) 7 - ___________- Strontium-90, dissolved. Chemical separation Uranium 8 ________________--------- and precipitation method (R-1160-76) 59 Collection and treatment of samples 9 __- -------- References ___________________________ 62 Calculations of radionuclide concentrations -- 11 Glossary _____________________-_--__---__-14 Tritium. Liquid scintillation method, Denver Selected references ______________________- 14 lab (R-1171-76) ______________________- 63 Principles of radioactivity, nuclear instru- Reference ____________________________ 66 mentation ___________________-------14 Tritium. Liquid scintillation method, Reston Compilations of data on radioactivity and lab (R-1173-76) _______________________ 67 radiochemistry _ _ ___ _ _ __ __ -- ___ ---- - - 14 References ___________________________ 71 Radioactivity in the environment ______ 15 Tritium. Electrolytic enrichment-liquid scin- Radioisotope methods in hydrology ______ 15 tillation method, Denver lab (R-1172-76) - 73 Radiochemical analytical methods ______ 15 Refepences ______-____________________ 78 15 Radioactivity regulations and safety ____ Tritium. Electrolytic enrichmenGliquid scin- References ____________-_-____------------16 79 tillation method, Reston lab (R-1174-76) _ Carbon-14, dissolved, apparent age. Liquid References ___________________________ 81 scintillation method, Denver lab (R-1100- Uranium, dissolved. Fluorometric method- 76) ____r________________~_~_~~~~~~~~~-17 direct (R-1180-76) 83 References 22 ..................... ___________________________ References 88 Cesium-137 and cesium-134, dissolved. Inor- ______________________--__- ganic ion-exchange method-gamma count- Uranium, dissolved. Fluorometric method4x- ing (R-1110-76) ___________________----23 traction procedure (R-1181-76) _________ 89 References ___________________________ 25 References __________________________- 92 Radiocesium, dissolved, as cesium-137. Inor- Uranium, dissolved, isotopic ratios. Alpha ganic ion-exchange method-beta counting spectrometry-chemical separation (R- (R-1111-76) ____________________-------27 1182-76) ___________-_---_-------------93 Reference ____________________--------28 Reference ____________________________ 95 V VI CONTENTS FIGURES Page 1. In-growth and decay of a daughter nuclide, significant time intervals --__ 13 2. Apparatus for collection of carbonates from a water sample _____________ -18 3. Vacuum line for preparation of acetylene and conversion to benzene ______ 19 4. Growth of bismuth-210 from pure lead-210 source ____________________- 36 5. Radon deemanation train and bubbler ______ _____________________-------44 6. Radon scintillation cell and housing ______________________~~~_~~~~~-~~-45 7. Apparatus for the distillation of ruthenium tetroxide _________________-__ 56 8. Ostlund electrolysis cell ______________________--_-__-_-_--___-_-____---75 9. Stevens apparatus for fusion and mixing of sample and flux in uranium determination ___________________________~_~______~_____~~__~~~~-~~~84 10. Platinum dish for use in Stevens apparatus _____________________-----_-85 11. Uranium caIibration curve ________________________________________---86 TABLES Page 1. Radon fraction (e-") remaining after radioactive decay for specified times - 48 2. Recommended sample volumes, minimum, and reduced volumes for isotopic uranium analysis __________________________________________--------94 METHODS FOR DETERMINATION OF RADIOACTIVE SUBSTANCES IN WATER AND FLUVIAL SEDIMENTS By L. 1. Thatcher and V. J. Janzer, U.S. Geological Survey, and K. W. Edwards, Colorado School of Mines Abstract referenced so that an experienced radio- Analytical methods for the determination of some chemist could set up the analytical method of the more important components of fission or neu- with reasonable assurance of success. Two tron adivation product radioactivity and of naturd exceptions are :the determination of tritium radioactivity found in water are reported. The re- by gas counting and the determination of port for each analytical method includes conditions for application of the method, a summary of the carbon-14.Because of the complexity of the method, interferences, required apparatus ’and reag- equipment and the extreme importance of ents, analytical procedures, calculations, reporting certain critical details in both the instru- of results, and estimation of precision. The fission mentation and operating procedure, any ab product isotopes considered are cesium-137, stnon- tempt to convey the fully detailed analytical tium-90, and ruthenium-106. The natural radioele- for ments and isotopes considered are uranium, lead-210, procedure direct duplication has a low radium-226, radium-228, tritium, and carbon-14. A probability fo’rsuccess. There is no substi- gross radioactivity survey method and a uranium tute for actual operating experience in labor- j isotope ratio method are given. When two analytical atories equipped for the gas-counting deter- methods are in routine use for an individual isotope, mination of tritium and the determination of both methods are reported with identification of the specific areas of application of each. Techniques for carbon-14. For the above reasons, the de- the collection and preservation of water samples to scriptions of these two analytical procedures be analyzed for radioactivity are discussed. concentrate on the principles and major op- erating conditions involved. In several analytical methods, reagents or Introduction equipment are cited by proprietary name. This is due to inadequate information on Purpose chemical composition on which to base a chemical name, or to special requirements This manual describes the analytical meth- known to be met by the cited reagent or ods used by the U.S. Geological Survey for equipment. In every case equivalent products the collection and analysis of water samples that meet requirements may be substituted. for radioactive substancw. The analytical No endorsement is intended. methods are intended for the radiochemist who applies his expertise to the analysis of water. Adequate grounding in the principles Organization and practice of radiochemistry is assumed. Each determination includes a section on Therefore, such subjects as nuclear instru- “Application,” “Summary of the method,” mentation, statistics, and radiation charac- “Interferences,” “Apparatus,”
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