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I. METHODS

Radioanalytical methods, sample preparation, sample dissolution, and instrument techniques.

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NEW: Sample Dissolution, Claude W. Sill and David S. Sill, Radioactivity & Radiochemistry, Vol. 6, No 2, 1995 pages 8-14

Extensive experimental evidence indicates that variable and incomplete sample dissolution is one of the major causes of the inaccurate results being obtained widely in radiochemical analysis. This conclusion is easily demonstrated by analysis of the residues remaining after the sample has been leached. The residue often contains a significant fraction of the radionuclide being determined. Three procedures involving high-temperature fusions are recommended that ensure complete dissolution of virtually all types of inorganic samples routinely and reliably. With a few unique exceptions encountered over many years of constant use, dissolution of the entire matrix has been so complete that a Tyndall beam could not be observed when the solution of the final fusion cake was examined with a flashlight in a darkened room. Complete material balance studies using radioactive tracers have also shown no significant losses of even the large terand quadrivalent radionuclides that could be attributed to incomplete dissolution of high specific-activity particles of the most refractory and intractable species. The recommended fusion procedures are no more hazardous, time-consuming or difficult than other procedures giving much less complete or reliable dissolution.

Fusion complete dissolution
NEW: Techniques of sample attack used in soil and mineral analysis – Phase I

Several techniques of sample attack for the determination of radioisotopes are reviewed. These techniques include 1) digestion with nitric or hydrochloric acid in Parr digestion bomb, 2) digestion with a mixture of nitric and hydrochloric acids, 3) digestion with a mixture of hydrofluoric, nitric and perchloric acids, and 4) fusion with sodium carbonate, potassium fluoride or alkali pyrosulfates. The effectiveness of these techniques to decompose various soils and minerals containing radioisotopes such as lead-210 uranium, thorium and radium-226 are discussed.

Soil Mineral Pb-210 Uranium thorium and radium-226
NEW: Simultaneous Determination of the Actinides in Small Environmental Samples

Simultaneous determination of all alpha activity has always been and continues to be a highly desirable option in radiochemical analysis. However, the usual practice of gross alpha counting samples of raw water evaporated to dryness in planchets, air dusts collected on filters, planchets full of soils, etc., and then reporting the results quantitatively is neither accurate nor reliable, since it is virtually impossible to determine the correct counting efficiency with which the count was actually made. Attempts to calibrate empirically for a given set of conditions are also of marginal value because of wide variability in the deposition patterns. Direct gross alpha counting of samples without chemical preparation is useful when the activity present is substantially higher than that from the natural activity in its surroundings, or when a rapid order-of-magnitude indication of alpha activity is desired. All too often the results of these screening methods are reported with precision and accuracy that they cannot possibly have. Even is excess alpha activity is indicated, a gross alpha count cannot distinguish between a man-made transuranium (TRU) radionuclide and a naturally occurring one. The current procedure provides a true total alpha while eliminating the problems just discussed.

actinides environmental samples
NEW: Determination of Actinides in Nuclear Wastes and Reference Materials for Ores and Mill Tailings, Claude W. Sill and David S. Sill, Waste Management, Vol 9, Issue 4, pp 219-229, 1989

(A fee may be required to access this article.)  Samples of siliceous solids up to 1 g were dissolved completely by successive fusions with potassium fluoride and pyrosulfate in platinum dishes in the presence of appropriate tracers. Samples which contaminate or react deleteriously with platinum were treated extensively with hydrofluoric and perchloric acids before fusion with pyrosulfate in glass. The pyrosulfate cake was dissolved in dilute hydrochloric acid and the actinides were precipitated isomorphously with barium sulfate. The barium sulfate was dissolved in alkaline ethylenediaminetetraacetic acid (EDTA), and the actinides were precipitated as the hydroxides, filtered on a membrane filter and analyzed in an alpha spectrometer. When necessary, the hydroxides were converted to fluorides in the presence of various oxidizing agents to obtain improved resolution and additional separations. Isotopes of all elements from thorium through curium can be determined in one sequential procedure. The procedure was simpler and faster than others available, with higher yields and greater reliability. Resolution of the subsequent alpha spectra was comparable to that obtained by electrodeposition. The results were reproduced with a relative standard deviation of 1 to 2%. The accuracy of the determination on standards was generally as good as the statistical uncertainty of the measurement permits. Some results of actinides in pond sediments, incinerator ash, baghouse dusts, and ion exchange resins are given.

Pyrosulfate fusion alpha spectrometer actinides
Rapid Method for Radium in Soil Incorporating the Fusion of Soil and Soil-Related Matrices with the Radioanalytical Counting Method for Environmental Remediation Following Radiological Incidents (pdf) (August 2012, 600-R-12-635)

Radium Fusion Soil Environmental Alpha Spectrometry
Beta-Particle Emitting Radionuclides, Procedure 43060S/22v100, Radiation Physics Division

Gross beta gross alpha liquid calibration Liquid scintillation counting
Rapid Determination of Gross Alpha and Gross Beta Activity in Ground Deposition and soil-like Solid Samples

gross alpha gross beta ground deposition soil environmental gas flow proportional counter
Low background gamma spectrometry for environmental radioactivity. T.M. Semkow, P.P. Parekh, C.D. Schwenker, A.J. Khan, A. Bari, J.F. Colaresi, O.K. Tench, G. David, W. Guryn. Appl. Rad. Isot. 57 (2002) 213

Gamma emitting radionuclides water; food gamma spectrometry;
Application of low-background gamma-ray spectrometry to monitor radioactivity in the environment and food. A.J. Khan, T.M. Semkow, S.E. Beach, D.K. Haines, C.J. Bradt, A. Bari, U.-F. Syed, M. Torres, J. Marrantino, M.E. Kitto, T. Menia, E. Fielman. Appl. Radiat. Isot. 90 (2014) 251.

(a fee may be required to obtain access to this article)

food gamma spectrometry
Gamma spectrometry of inhomogeneous samples using peak-ratio method. T.M. Semkow, L.T. Chu, A.G. Burn. J. Appl. Math. Phys. 9 (2021) 2641

soil environmental gamma spectrometry 152Eu signal detection theory hot particles bias
Multifarious application of well-type germanium detector. P.P. Parekh, T.M. Semkow, A. Bari, M.A. Torres, D.K. Haines, P.R. Harris, E.M. Fielman, M.E. Kitto. J. Radioanal. Nucl. Chem. 262 (2004) 317

environmental animal soil sediment drinking water gamma spectrometry 125I 129I 210Pb 228Ra 238U 239Pu 240Pu 241Pu well-type detector
Rapid and simultaneous detection of alpha/beta radioactivity in food by solid phase extraction liquid scintillation counting. Lin Z, Healey S, Wu Z

gross alpha gross beta 90Sr 90Y 239Pu 241Am food liquid scintillation counter
Rapid alpha spectroscopy of evaporated liquid residues for emergency response. Semkow TM, Khan AJ, Haines DK, Bari A. Health Phys. 2009 Apr;96(4):432-41.

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https://www.researchgate.net/publication/24191851_Rapid_alpha_spectroscopy_of_evaporated_liquid_residues_for_emergency_response (request full text pdf from authors)

241Am 239Pu 90Sr gross alpha gross beta food liquid scintillation counter gas proportional detector
Rapid radiochemical analysis of 131I in environmental samples using a well-type Ge-detector. Parekh, P., Bari, A. & Harris, P. Journal of Radioanalytical and Nuclear Chemistry 256, 225–230 (2003).

(a fee may be required to obtain access to this article) 

https://www.researchgate.net/publication/226921743_Rapid_radiochemical_analysis_of_131I_in_environmental_samples_using_a_well-type_Ge-detector (request full text from authors)

131I iodine131 iodine Human Thyroid Milk Food HPGe Detector Counting
Homogenization of food samples for gamma spectrometry using protease. Nishikawa, K., Bari, A., Khan, A.J. et al. J Radioanal Nucl Chem 318, 401–406 (2018).

(a fee may be required to obtain access to this article) 

https://www.researchgate.net/publication/315494639_Homogenization_of_Food_Samples_for_Gamma_Spectrometry_Using_TMAH_and_Enzymatic_Digestion (request full-text pdf from authors)

7Be 60Co 137Cs 131I 241Am plant food gamma spectrometry
Homogenization of food samples for gamma spectrometry using tetramethylammonium hydroxide and enzymatic digestion. Nishikawa, K., Bari, A., Khan, A.J. et al. J Radioanal Nucl Chem 314, 859–870 (2017).

60Co 134Cs 137Cs 131I 241Am food gamma spectrometry
Radiochemical analysis of a wide range of 131I activities in water and milk using well-type germanium detector. Li, X., Semkow, T.M., Bradt, C.J. et al. J Radioanal Nucl Chem 313, 197–206 (2017). https://doi.org/10.1007/s10967-017-5292-0

(a fee may be required to obtain access to this article)

131I 129I water milk food gamma spectrometry
Rapid screening of radioactivity in food for emergency response. Bari A, Khan AJ, Semkow TM, Syed UF, Roselan A, Haines DK, Roth G, West L, Arndt M. Appl Radiat Isot. 2011 Jun;69(6):834-43. doi: 10.1016/j.apradiso.2011.02.022 . Epub 2011 Feb 17. PMID: 21388817

(a fee may be required to obtain access to this article)

Gross Alpha Gross Beta 60Co 90Sr 137Cs 131I 241Am Food Gas Proportional Counter
Rapid Determination of Thorium in Urine by Quadrupole Inductively Coupled Plasma Mass Spectrometry (Q-ICP-MS). Liu, Y.; Xiao, G.; Jones, R. L. J Radioanal Nucl Chem 2022. https://doi.org/10.1007/s10967-022-08408-9 (a fee may be required to obtain access to this article)

Thorium Urine clinical inductively coupled plasma mass spectrometry
Limit of Detection Comparison on Urine Gross Alpha/Beta, H-3, and P-32 Analysis between Different Liquid Scintillation Counters. Piraner, O.; Jones, R. L. J Radioanal Nucl Chem 2021, 330 (1), 381–384

Gross Alpha/Beta tritium phosphorus-32 Urine clinical liquid scintillation counting
Urine Strontium-90 (Sr-90) Manual and Automated Pre-Analytical Separation Followed by Liquid Scintillation Counting. Piraner, O.; Jones, R. L. J Radioanal Nucl Chem 2021, 329 (1), 383–390

strontium-90 urine clinical liquid scintillation counter
Determination of 239Pu in Urine by Sector Field Inductively Coupled Plasma Mass Spectrometry (SF-ICP-MS) Using an Automated Offline Sample Preparation Technique. Xiao, G.; Jones, R. L. J Radioanal Nucl Chem 2021, 328 (1), 277–287

plutonium-239 urine clinical Sector Field Inductively Coupled Plasma Mass Spectrometry
Rapid HPGe Well Detector Gamma Bioassay of 137Cs, 60Co, and 192Ir Method. Button, J.; Jones, R. L. Applied Radiation and Isotopes 2021, 175, 109824

137Cs 60Co 192Ir urine clinical HPGe gamma spectroscopy
Urine Gross Alpha/Beta Bioassay Method Development Using Liquid Scintillation Counting Techniques. Piraner, O.; Jones, R. L. J Radioanal Nucl Chem 2021, 327 (1), 513–523

gross alpha/beta urine clinical liquid scintillation counting
Determination of 226Ra in Urine Using Triple Quadrupole Inductively Coupled Plasma Mass Spectrometry. Xiao, G.; Liu, Y.; Jones, R. L. Radiation Protection Dosimetry 2020, 191 (4), 391–399

Radium-226 urine clinical inductively coupled plasma mass spectrometry
Determination of 237Np and 239Pu in Urine Using Sector Field Inductively Coupled Plasma Mass Spectrometry (SF-ICP-MS). Xiao, G.; Liu, Y.; Jones, R. L. J Radioanal Nucl Chem 2020, 324 (2), 887–896

237Np 239Pu Urine clinical Sector Field inductively coupled plasma mass spectrometer
Determination of 234U/238U, 235U/238U and 236U/238U Isotope Ratios in Urine Using Sector Field Inductively Coupled Plasma Mass Spectrometry. Xiao, G.; Jones, R. L.; Saunders, D.; Caldwell, K. L. Radiation Protection Dosimetry 2014, 162 (4), 618–624

234U/238U 235U/238U 236U/238U urine clinical inductively coupled plasma mass spectrometer
Determination of 241Am in Urine Using Sector Field Inductively Coupled Plasma Mass Spectrometry (SF-ICP-MS). Xiao, G.; Saunders, D.; Jones, R. L.; Caldwell, K. L. J Radioanal Nucl Chem 2014, 301 (1), 285–291.

Americium-241 urine clinical inductively coupled plasma mass spectrometer
Selected Analytical Methods for Environmental Remediation and Recovery (SAM) 2017 (pdf) (September

Gross Alpha Gross Beta Americium-241 Californium-252 Cesium-137 Cobalt-60 Curium-244 Europium-154 Indium-111 Iodine-125 Iodine-131 Iridium-192 Molybdenum-99 Neptunium-237 Neptunium-239 Phosphorus-32 Plutonium-238 Plutonium-239 Polonium-210 Radium-223 Radium-226 Rhenium-188 Rubidium-82 Ruthenium-103 Ruthenium-106 Selenium-75 Strontium-89 Strontium-90 Technetium-99 Technetium-99m Thorium-227 Thorium-228 Thorium-230 Thorium-232 Tritium Uranium-234 Uranium-235 Uranium-238
Rapid Radiochemical Method for Curium-244 in Water Samples for Environmental Remediation Following Radiological Incidents (pdf) (May 2017, EPA 402-S17-001)

Curium-244 water environmental alpha spectrometry
Rapid Radiochemical Method for Curium- 244 in Air Particulate Filters, Swipes and Soil for Environmental Remediation Following Radiological Incidents (pdf) (May 2017, EPA 402-S17-004)

curium-244 filters swipes soil environmental alpha spectrometry
Improved Rapid Radiochemical Method for Radium-226 in Building Materials for Environmental Remediation Following Radiological Incidents (pdf) (May 2017, EPA 402-S17-002)

Radium-226 asphalt shingles limestone granite environmental alpha spectrometry
Rapid Radiochemical Method for Californium-252 in Water, Air Particulate Filters, Swipes, and Soils for Environmental Remediation Following Radiological Incidents (pdf) (May 2017, EPA 402-S17-003)

californium-252 water filters soil environmental alpha spectrometry
Rapid Method for Sodium Hydroxide Fusion of Asphalt Roofing Material Matrices Prior to Americium, Plutonium, Strontium, Radium, and Uranium Analyses (pdf) (May 2017, EPA 402-R-16-003)

americium plutonium strontium radium uranium fusion Asphalt roofing environmental muffle furnace
Rapid Method for Sodium Hydroxide Fusion of Asphalt Matrices Prior to Americium, Plutonium, Strontium, Radium, and Uranium Analyses (pdf) (May 2017, EPA 402-R-16-001)

americium plutonium strontium radium uranium fusion Asphalt environmental muffle furnace
Rapid Method for Sodium Hydroxide Fusion of Concrete and Brick Matrices Prior to Americium, Plutonium, Strontium, Radium, and Uranium Analyses for Environmental Remediation Following Radiological Incidents (pdf) (April 2014, 402-R-14-004)

americium plutonium strontium radium uranium fusion concrete brick environmental muffle furnace
Rapid Radiochemical Method for Isotopic Uranium in Building Materials for Environmental Remediation Following Radiological Incidents (pdf) (April 2014, 402-R-14-005)

Uranium-238 uranium-235 uranium-234 building materials environmental alpha spectrometry
Rapid Radiochemical Method for Total Radiostrontium (Sr-90) In Building Materials for Environmental Remediation Following Radiological Incidents (pdf) (April 2014, 402-R-14-001)

strontium building materials environmental gas flow proportional
Rapid Radiochemical Method for Radium-226 in Building Materials for Environmental Remediation Following Radiological Incidents (pdf) (April 2014, 402-R-14-002)

Radium-226 building materials environmental alpha spectrometry
Rapid Radiochemical Method for Plutonium-238 and Plutonium-239/240 in Building Materials for Environmental Remediation Following Radiological Incidents (pdf) (April 2014, 402-R-14-006)

Plutonium-238 plutonium-239/240 fusion building materials environmental alpha spectrometry
Rapid Radiochemical Method for Americium-241 in Building Materials for Environmental Remediation Following Radiological Incidents (pdf) (April 2014, 402-R-14-007)

Americium-241 building materials environmental alpha spectrometry
Rapid Method for Sodium Hydroxide/Sodium Peroxide Fusion of Radioisotope Thermoelectric Generator Materials in Water and Air Filter Matrices Prior to Plutonium Analyses for Environmental Remediation Following Radiological Incidents (pdf) (April 2014, 402-R14-003)

Plutonium-238 Radioisotope Thermoelectric Generator fusion water air filters environmental alpha spectrometry
Rapid Method for Fusion of Soil and Soil-Related Matrices Prior to Americium, Plutonium, and Uranium Analyses for Environmental Remediation Following Radiological Incidents (pdf) (August 2012, 600-R-12-636/7/8)

Radium fusion soil environmental alpha spectrometry
Rapid Method for Sodium Carbonate Fusion of Glass-Fiber and Organic/Polymeric Composition Filters and Swipes Prior to Isotopic Uranium, Plutonium, Americium, Strontium, and Radium Analyses for Environmental Remediation Following Homeland Security Events (pdf) (October 2012, 402-R-12-008)

Uranium Plutonium Americium Strontium Radium fusion filters environmental Fisher blast burner or Meeker burner
Rapid Radiochemical Methods for Selected Radionuclides in Water for Environmental Restoration Following Homeland Security Events (pdf) (February 2010, 402-R-10-001)

Americium-241 Plutonium-238 Plutonium-239/240 Radium-226 strontium uranium-238 uranium-235 uranium-234 water environmental alpha spectrometry gas-flow proportional counter
Rapid Radiochemical Method for Isotopic Uranium in Water for Environmental Remediation Following Homeland Security Events (pdf) (October 2011, 402-R-10-001e)

Uranium-238 uranium-235 uranium-234 water environmental alpha spectrometry
Rapid Radiochemical Method for Total Radiostrontium (Sr-90) In Water for Environmental Remediation Following Homeland Security Events (pdf) (October 2011, 402-R-10-001d)

Strontium water environmental gas flow proportional counter
Rapid Radiochemical Method for Radium-226 in Water for Environmental Remediation Following Homeland Security Events (pdf) (October 2011, 402-R-10-001c)

Radium-226 water environmental alpha spectrometry
Rapid Radiochemical Method for Phosphorus-32 in Water for Environmental Remediation Following Homeland Security Events (pdf) (November 2011, 600-R-11-181)

Phosphorus-32 Water Environmental liquid scintillation counting inductively coupled plasma-atomic emission spectrometry
Rapid Radiochemical Method for Plutonium-238 and Plutonium-239/240 in Water for Environmental Remediation Following Homeland Security Events (pdf) (October 2011, 402-R-10-001b)I.

Plutonium-238 Plutonium-239/240 Water Environmental alpha spectrometry
Rapid Radiochemical Method for Americium-241 in Water for Environmental Remediation Following Homeland Security Events (pdf) (October 2011, 402-R-10-001a)

Americium-241 water environmental alpha spectrometry OR SPECTROSCOPY
Rapid Method for Sodium Carbonate Fusion of Soil and Soil-Related Matrices Prior to Strontium-90 Analyses for Environmental Remediation Following Radiological Incidents (pdf) (August 2012, 600-R-12-640)

Strontium-90 fusion soil environmental muffle furnace
Rapid Method for Acid Digestion of Glass-Fiber and Organic/Polymeric Composition Filters and Swipes Prior to Isotopic Uranium, Plutonium, Americium, Strontium, and Radium Analyses for Environmental Remediation Following Homeland Security Events (pdf) (October 2012, 402-R-12-009)

Uranium (U) plutonium (Pu) americium (Am) strontium radium filters swipes environmental muffle furnace
Rapid Method for Sodium Hydroxide Fusion of Limestone Matrices Prior to Americium, Plutonium, Strontium, Radium, and Uranium Analyses for Environmental Remediation Following Radiological Incidents (pdf) (August 2018, 402-R-18-002)

americium plutonium strontium radium uranium fusion limestone environmental muffle furnace
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