Problems in the determination of plutonium in bioassay and environmental analysis

Veselsky, J. C.

doi:10.1016/s0003-2670(01)82288-1

Cited by 24 publications

(4 citation statements)

References 52 publications

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“…As an additional check, 140 routine urine samples were taken and analyzed by each method after the samples were divided equally. Also, 54 QC samples were analyzed by the oxalate method and 12 QC samples by the AEP method. The average recovery of the 242Pu spike for 194 samples by the oxalate method was 90.5% with a standard deviation of ±10.1 and a range of 43-111%.…”

Section: Resultsmentioning

confidence: 99%

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Separation of plutonium in urine without sample ashing for determination by .alpha.-spectrometry

Kressin¹

1981

Anal. Chem.

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Present methods for the analysis of plutonlum In urine requlre ashing the organic constituents of the sample, a time-conmlng procedure and a major source of error. A method was developed to quantitatively separate 25 fCi of plutonium directly from 800 cm3 of urlne by copreclpltatlon with calcium oxalate. Wlthout ashlng, the oxalate precipitate Is directly dlssoived in 7.2 M HNO, and the plutonium Is Isolated by anion exchange, electrodeposited, and then measured by cu-spectrometry. The results are in excellent agreement with results obtained by exlstlng procedures, and for 194 samples the average recovery of the plutonlum tracer was 91 % with a standard deviation of f10. The average recovery of the plutonium Isotope in quality control samples was 101 % when corrected for the 242Pu tracer recovery.The potential health hazards of plutonium have been recognized, and it has been our practice at the Los Alamos National Laboratory to monitor workers for exposure to plutonium (1). One of our methods is to analyze a worker's urine, and the method must be capable of detecting 25 fCi (0.056 dpm) in 800 cm3 of urine in order that the health protection controls can be properly evaluated. Instruments have been developed to accurately detect 25 fci of plutonium, but these instruments cannot detect 25 fCi of plutonium in a urine matrix. Therefore, the problem is the separation and isolation of 25 fCi of plutonium from a liter of urine. White, Handler, and Smith (2) reported the urine of a normal adult over a 24-h period to have the constituents listed in Table I. The composition of samples will vary widely due to illness, medication, or strenuous exercise, and although freshly voided urine may also appear clear, it may contain proteins and cells from the lining of the genitourinary tract.To achieve the required detection limit in urine with such a large variation of cellular elements and mucus, present methods (3-11) eliminate the organic components by wet or dry ashing. In addition to being very time-consuming, ashing is one of the major causes of erratic results. Veselsky (12) presents a review of the problems of various types of bioassay samples. Lisk (13) points out that sample preparation, ashing, element isolation, and concentration are usually the most critical steps in trace element analysis of biological samples. Gorsuch (14) presents a comprehensive review of sample ashing and the recovery or losses caused by different ashing procedures, temperatures, and other operating parameters for the destruction of organic matter for trace element analysis.

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Section: Resultsmentioning

confidence: 99%

“…In addition to being very time-consuming, ashing is one of the major causes of erratic results. Veselsky (12) presents a review of the problems of various types of bioassay samples. Lisk (13) points out that sample preparation, ashing, element isolation, and concentration are usually the most critical steps in trace element analysis of biological samples.…”

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confidence: 99%

Separation of plutonium in urine without sample ashing for determination by .alpha.-spectrometry

Kressin¹

1981

Anal. Chem.

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“…Various techniques for preparing radioactive sources have been reviewed [3,7], among which electrodeposition, in which a radioactive material dissolved in an electrolyte solution is electrodeposited on a cathode (source support) by passing an electric current, is commonly used to prepare ultrathin solid radioactive sources [9][10][11][12][13][14][15][16][17]. The advantages of this source preparation method include high deposition yields (99.8%) and high qualities of the sources obtained with simple and inexpensive equipment [7], which make it the most common method of radioactive source preparation.…”

Section: Introductionmentioning

confidence: 99%

Preparation of alpha sources using magnetohydrodynamic electrodeposition for radionuclide metrology

Panta

Farmer

Johnson

et al. 2010

Journal of Colloid and Interface Science

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“…Of all the transuranium elements, plutonium has been studied most extensively and numerous procedures have been reported for its determination [1][2][3][4][5][6][7][8][9], Current techniques for the determination of plutonium trace level are mainly radiochemical methods (a-spectrometry, y spectrometry, liquid scintillation counting) carried out after chemical preparation of the samples. Interest has also tumed to various mass spectrometry techniques (ICP-MS [10,11], TIMS [12,13]), but those methods are not really adapted for a matrix where uranium is the principal constituent because of isobaric interfering effects.…”

Section: Introductionmentioning

confidence: 99%

Alpha Spectrometric Determination of Trace Level of ^239-240Pu and ²³⁸Pu Uranium Compounds and Solutions

1999

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Plutonium / Uranium / Anion-exchange chromatography / Extraction chromatography / Alpha spectrometry / ElectrodepositionSummary An accurate and reliable analytical method has been developed for the measurement of low-level of plutonium nuclides (^''Pu, 239 -24oj>y^ in uranium Compounds and solutions by alpha spectrometry, with emphasis on the purification of plutonium nuclides from uranium isotopes and their a emitting decay radionuclides. The method mainly consists of Chromatographie separations. TWo steps of purification are necessary, the first one using a REILLEX™ HPQ (anion-exchange macroporous resin) Chromatographie column and the second one consisting in extraction chromatography with trioctylamine (TOA). ^"Pu was used as isotopic tracer: plutonium recovery yields for the entire process were found dose to 90% and the minimum detectable Pu activity was about lOmBq/sample for a counting time of 5 hours using a grid Chamber, after the implementation of a Separation with a good decontamination factor (higher than 10^) of plutonium vs. uranium. For a lower detection limit, it is necessary to increase the counting time.

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Problems in the determination of plutonium in bioassay and environmental analysis

Cited by 24 publications

References 52 publications

Separation of plutonium in urine without sample ashing for determination by .alpha.-spectrometry

Separation of plutonium in urine without sample ashing for determination by .alpha.-spectrometry

Preparation of alpha sources using magnetohydrodynamic electrodeposition for radionuclide metrology

Alpha Spectrometric Determination of Trace Level of ^239-240Pu and ²³⁸Pu Uranium Compounds and Solutions

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Problems in the determination of plutonium in bioassay and environmental analysis

Cited by 24 publications

References 52 publications

Separation of plutonium in urine without sample ashing for determination by .alpha.-spectrometry

Separation of plutonium in urine without sample ashing for determination by .alpha.-spectrometry

Preparation of alpha sources using magnetohydrodynamic electrodeposition for radionuclide metrology

Alpha Spectrometric Determination of Trace Level of 239-240Pu and 238Pu Uranium Compounds and Solutions

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Alpha Spectrometric Determination of Trace Level of ^239-240Pu and ²³⁸Pu Uranium Compounds and Solutions