Simultaneous determination of210Bi and210Po on pine needles by solvent extraction and liquid scintillation counting

A determination procedure has been developed for²¹⁰Bi and²¹⁰Po in environmental samples and was applied for pine needles. Bismuth-210 and²¹⁰Po separated from the parent nuclide²¹⁰Pb as BiOCl precipitate were extracted simultaneously by TOPO/toluene containing PPO and POPOP. The separation of²¹⁰Bi and²¹⁰Po from²¹⁰Pb was almost satisfactory. The activity of²¹⁰Bi+²¹⁰Po in the TOPO/toluene was measured periodically by liquid scintillation counting for about 20 days after separation. The time course of the decreasing pattern of the activity was determined by the initial activity ratio²¹⁰Po/²¹⁰Bi. The decreasing pattern of the activity was compared with theoretical patterns, and best estimates for²¹⁰Po and²¹⁰Bi were obtained by non-linear least-squares fitting. The activities of²¹⁰Bi and²¹⁰Po were determined for one-year and two-year old pine needles fro the same pine tree, and weathering half-time and deposition rate of these nuclides was discussed.     

Evaluation of measurement uncertainty in the determination of 210Pb and 210Po using beta counting and alpha spectrometry

 Measurement uncertainties in the determination of ²¹⁰Pb and ²¹⁰Po in Reference Material IAEA-300 (Baltic Sea Sediment) were evaluated. ²¹⁰Pb and ²¹⁰Po were separated from the matrix using an Sr resin column. The chemical yield of ²¹⁰Pb was determined gravimetrically in PbSO₄ form. Precipitation was followed by beta proportional counting after ²¹⁰Bi ingrowth. ²¹⁰Po was determined by alpha spectrometry after its spontaneous deposition on a Cu planchet. The major source of uncertainty was identified as the statistical counting uncertainty, which was also expected and is almost impossible to reduce without extension of the time required for an analysis. The expanded uncertainties were determined as 7.4% and 12.2% for ²¹⁰Pb and ²¹⁰Po, respectively. Received: 3 September 2002 Accepted: 3 December 2002 Acknowledgement This work was financially supported by Ministry of Education, Science and Sport, Republic of Slovenia (Project group PO-0106–0532). Presented at CERMM-3, Central European Reference Materials and Measurements Conference: The function of reference materials in the measurement process, May 30–June 1, 2002, Rogaška Slatina, Slovenia Correspondence to P. Vreˇcek     

Separation of the radioelements210Pb−210Bi−210Po by spontaneous deposition onto noble metals and verification by Cherenkov and liquid scintillation counting

A method for the separation of²¹⁰Pb,²¹⁰Bi and²¹⁰Po using spontaneous deposition has been developed. The²¹⁰Bi and²¹⁰Po are simultaneously removed by deposition onto nickel foil (copper and tin could also be used but less effectively) while the²¹⁰Po is separated from²¹⁰Bi, after dissolution of the nickel foil, by deposition onto silver foil. The effectiveness of each separation was evaluated by adding aliquot portions of each solution to a cocktail and counting with a liquid scintillation counter. Water was used as the medium to observe the Cherenkov count of the sample solution.     

Radiochemical determination of210Po and210Pb in water

A method for²¹⁰Po and²¹⁰Pb determination in water samples is described. The nuclides are concentrated, in presence of added²⁰⁸Po and lead carrier, by evaporation. Then the polonium is plated electroless from the acidic solution on a copper planchet and measured by alpha spectrometry.²¹⁰Pb separation from the other isotopes is based on the solutility of PbSO₄ in citrate.²¹⁰Pb content is determined by measuring the activity of its daughter²¹⁰Bi. The critical steps in the isolation of lead have been examined and discussed.     

Quantification of measurement uncertainty in the sequential determination of <Superscript>210</Superscript>Pb and <Superscript>210</Superscript>Po by liquid scintillation counting and alpha-particle spectrometry

Methodologies for the quantification of measurement uncertainties associated with the determination of ²¹⁰Pb- and ²¹⁰Po-specific activities by liquid scintillation counting (LSC) and alpha-particle spectrometry are presented, and are demonstrated using the soil reference material IAEA-326. Major contributors to the combined uncertainty associated with the measurement result of ²¹⁰Pb were the uncertainties of net count rates in the ²¹⁰Pb energy region of the sample spectrum and in the ²¹⁰Bi energy region of the blank spectrum. The predominant sources of uncertainty in the measurement of ²¹⁰Po were the uncertainties of net count rates in the regions of interest of ²⁰⁹Po and ²¹⁰Po. The relative standard uncertainty of ²¹⁰Po exponentially increases with the time interval between the sampling date and the separation date of Po, and this effect is strongly dependent on the ²¹⁰Po/²¹⁰Pb activity ratio. When the specific activity of ²¹⁰Pb is much higher than that of ²¹⁰Po in the sample, the relative standard uncertainty of the ²¹⁰Po determination increases significantly within a short time interval between the sampling date (or reference date) and the separation date of Po in samples.     

A practical and accurate method for the determination of 234Th simultaneously with 210Po and 210Pb in seawater

A practical technique has been developed for the determinations of (234)Th simultaneously with (210)Po and (210)Pb in seawater samples, which greatly simplifies the on-board chemical procedures and enables an accurate correction of (234)Th ingrowth. A unique feature of this technique lies in the exact determination of co-precipitated (238)U following Fe(OH)(3) precipitation which leads to an exact correction of ingrown (234)Th between Fe(OH)(3) precipitation and U/Th separation. Such a correction eliminates several cumbersome on-board chemistry steps (such as Po plating, Fe(2+) oxidation, and 9 N HCl anion exchange) required in regular procedures to eliminate the (234)Th ingrowth. The total time required for on-board sample treatment (spike equilibration, Fe (OH)(3) co-precipitation and filtration) could be less than 10 h which significantly increases the sample processing efficiency and data throughput.     

The role of Cherenkov and liquid scintilation counting in evaluating the anion-exchange separation of210Pb−210Bi−210Po

Using as eluent a sequence of 3M HCl, 12M HCl, and 8M HNO₃, a mixture of²¹⁰Pb,²¹⁰Bi, and²¹⁰Po may be clearly separated on a column of Dowex 1×2−100 anion exchange resin. A Cherenkov count in H₂O and the variation in count rate with time confirm that the nuclides emerge in the order²¹⁰Pb→²¹⁰Bi→²¹⁰Po. If 12M HCl is replaced by 1.5M H₂SO₄/2.3 M Na₂SO₄, a clean separation also results, but recovery of²¹⁰Po becomes considerably more difficult. All three nuclides are readily detectable by liquid scintillation counting, with the efficiency for²¹⁰Pb in the 60–70% range. The Cherenkov aqueous counting efficiency for²¹⁰Bi is ∼14–15%.     

Absolute liquid scintillation counting of35S and45Ca using a modified integral counting method

The disintegration rates of³⁵S and⁴⁵Ca samples were determined by the modified integral counting method, which extrapolates the integral count rate to the zero detection threshold of a liquid scintillation spectrometer. The agreement between the extrapolated value and the standardized disintegration rate of the sample is very satisfactory.     

Improved method for the determination of the cortisol production rate using high-performance liquid chromatography and liquid scintillation counting

Two new methods for the determination of the cortisol production rate using reversed-phase high-performance liquid chromatography are described. One uses ultraviolet detection at 205 nm, the other on-line post-column derivatization with benzamidine, followed by fluorimetric detection. The specific activity of tetrahydrocortisol and tetrahydrocortisone in urine from patients who had received tritium-labelled cortisol was determined by the indicated methods, followed by fraction collection and liquid scintillation counting. The post-column reaction detection procedure was superior to ultraviolet detection, both in selectivity and analysis time. Intra- and inter-assay variance of the post-column reaction detection procedure were 3.7 and 4.7%, respectively. A good correlation (r = 0.99) was obtained between values determined by this procedure and by a thin-layer chromatographic procedure.     

Determination of 210Pb by measurement of 210Pb and its progenies using a liquid scintillation counter

Journal of Radioanalytical and Nuclear Chemistry - Lead-210 is a useful tracer in environmental studies for a wide range of applications, particularly in atmospheric research and geochronology....     

A novel method for the simultaneous determination of125I and14C activities using liquid scintillation counting

The viability of a dual label liquid scintillation technique has been investigated. To avoid the need for two procedures, gamma counting for¹²⁵Iodine (¹²⁵I) and liquid scintillation counting for¹⁴C. Since the¹²⁵I spectrum covers almost as wide a range of pulse heights as¹⁴C, conventional dual label methods would result in very low¹⁴C counting efficiencies. The conventional dual label technique has ben modified to increase the¹⁴C counting efficiency and to accomodate the consequent additional spillover of¹²⁵I counts into the upper window. This dual label technique has been applied to the determination of¹²⁵I and¹⁴C activities in blood samples. The accuracy of the method has been tested, and its advantages and limitations are discussed.     

210Pb and its progenies in phosphoric acid: Significance for low level determinations using liquid scintillation counting with extractive cocktails

When measuring²¹⁰Pb via its progenies using the extractive cocktail Polex^TM, the sample must be transferred to a phosphate system. When measuring low level samples, care has to be taken in the choise of the phosphoric acid used, as it may contain rather large amounts of²¹⁰Pb. Typical activity concentrations for products of different manufacturers are given.     

A rapid method for the separation of 210 Po from 210 Pb by TIOA extraction

A rapid method for the separation of ²¹⁰ Po from ²¹⁰ Pb was developed utilizing extraction of triisooctylamine (TIOA)/xylenein HCl+H₂O₂ medium. Polonium in the form of PoCl ₆ ²– was extracted into TIOA phase and ²¹⁰Pb remains in the aqueous phase. Lead-²¹⁰ was determined by -countingof its granddaughter, ²¹⁰ Po ingrown from ²¹⁰ Pb forsome period of time. Distribution of ²¹⁰ Po and ²¹⁰Pb in TIOA and aqueous phases was investigated in various concentrations ofHCl media. Hydrogen peroxide was used to further decompose organic matterand to remove sulfur to prevent its deposition on the silver disc. The improvedprocedure resulted in a good chemical yield (80–95%) and a good á-resolution.     

Determination of 90Sr and 210Pb in deer bone samples by liquid scintillation counting after ion-exchange procedures

This work describes a procedure for the isolation of ⁹⁰Sr and ²¹⁰Pb from deer bones by anion exchange methods and their sequential measurement by LSC. To prevent collection of Pb on the Sr·Spec^® resin we first separated Pb on a Dowex anion exchange column. Sr, which is not held back on the Dowex column, was then purified using Sr·Spec^® resin: first Ca and the Ra isotopes were eluted with 3 M HNO₃ and then Sr was eluted with distilled water. With this 2-steps procedure pure ²¹⁰Pb and ⁹⁰Sr spectra can be achieved. The chemical yield of both steps was determined by ICP-MS. Our ⁹⁰Sr results show satisfying agreement with data obtained by a shorter Sr·Spec^® method and also by the “classical” ⁹⁰Sr determination using fuming nitric acid. Also ²¹⁰Pb results were checked by re-measuring bone samples with already known ²¹⁰Pb activities. Further our method was verified on the reference sample IAEA-A-12.     

Development of a method for the determination of 226Ra by liquid scintillation counting

Liquid scintillation counting has not been widely applied to a-particle detection because of its poor energy resolution and variable background. In the present work, a time saving and reasonably accurate method for determination of ²²⁶Ra in water has been developed, using liquid scintillation spectrometry and pulse-shape analysis. The effect of three levels of chemical quench on the spillover of alpha interactions into the beta window and vice versa was assessed. The advantages of liquid scintillation in comparison with other methods (radon emanation) for determination of ²²⁶Ra are the high counting efficiency (~100%) and the easier sample preparation, with no need for sample preconcentration.     

Radiometric determination of trace amounts of zinc using liquid scintillation counting

A sensitive and selective radiometric method of substoichiometric isotope dilution analysis for the determination of trace amounts of zinc is described. The activity of (65)Zn used as a tracer in this method was measured by liquid scintillation counting and its counting efficiency was found to be 76+/-2.7%. The method is based on the extraction of the ion-association complex of zinc from thiocyanate medium at pH 7.9 using substoichiometric amount of Aliquat-336 in toluene. The method is sensitive to 20 ng of Zn(II) in an aqueous phase volume of up to 15 ml and its reliability was tested by applying it to a certified reference material-magnesium alloy and pharmaceutical samples.     

Levels of 210Po and 210Pb in cigars

²¹⁰Po and ²¹⁰Pb concentrations have been determined in 58 cigar brands manufactured in 11 countries. Cuban and American cigars showed the lowest ²¹⁰Po content. The mean levels of ²¹⁰Po in Brazilian, European and Dominican cigars were almost identical and somewhat lower than the levels observed for cigars from other Latin American countries. Cuban, American and European cigars contained low levels of ²¹⁰Pb. Cigars from the remaining countries contained twice as much ²¹⁰Pb. The mean ²¹⁰Po/²¹⁰Pb ratio showed an excess of polonium. In the case of a one cigar-a-day smoker, the calculated annual absorbed dose due to ²¹⁰Po is -16 mGy.