Determination of U/U atom ratio in uranium samples using liquid scintillation counting (LSC)

A correlation has been developed for the determination of ²³⁵U/²³⁸U atom ratio in uranium samples using liquid scintillation counting (LSC). The ²³⁵U/²³⁸U atom ratio determined by thermal ionization mass spectrometry (TIMS) was correlated to the ratio of (i) α-count rate and (ii) Cerenkov count rate due to ^234mPa in the sample; both measured by LSC. This correlation is linear over the range of ²³⁵U/²³⁸U atom ratio encountered in the nuclear fuel samples, i.e. the low enriched uranium (LEU) samples with ²³⁵U < 20 atom%. The methodology based on this correlation will be useful for the quick determination and verification of ²³⁵U/²³⁸U atom ratios in fuel samples using cost effective technique of LSC.     

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.     

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.     

Fast determination of indoor radon (<Superscript>222</Superscript>Rn) concentration using liquid scintillation counting

The indoor ²²²Rn radionuclide was directly absorbed in typical 20 ml glass scintillation vials by passing ?3 dm³ of ambient air through 16 ml of water-immiscible non-volataile scintillation cocktail Ultima-Gold F for 10 min. The activity of radon and its two α-emitting daughters: ²¹⁸Po and ²¹⁴Po, was determined with the BetaScout low-background liquid scintillation counter. The limit of ²²²Rn detection is 9 Bq/m³, and the quantification limit with 20% relative accuracy is 28 Bq/m³. The results of the indoor Rn measurement in different houses showed good consistency with results obtained from a Sarad EQF 3220 device.     

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.     

A modified method for the sequential determination of 210Po and 210Pb in Ca-rich material using liquid scintillation counting

This research describes methods for the sequential determination of ²¹⁰Pb and ²¹⁰Po activity concentrations in Ca-rich ash samples collected from oil shale-fired power plants in Estonia. The procedure involves digestion of Ca-rich ash samples in a microwave digestion system, radiochemical separation of ²¹⁰Pb and ²¹⁰Po and their measurements. All samples, blanks and standards were measured by liquid scintillation counting (Quantulus 1220). The method was tested using IAEA (International Atomic Energy Agency) RGU-1 and IAEA-444 reference materials. Spectral calibration/peak identification which included the optimization of α/β discrimination system (pulse shape analyser), and recovery have been made by ²⁰⁹Po and ²¹⁰Pb standard solutions.

     

Method validation and verification in liquid scintillation counting using the long-term uncertainty method (LTUM) on two decades of proficiency test data

Results from proficiency tests gathered over the past two decades by the laboratory for low level radioactivity measurements for liquid scintillation counting of ³H (184 results) and ¹⁴C (74 results) are used to verify the validated measurement methods used by the laboratory, in particular the estimated uncertainty budget of the method and its reproducibility and stability. A linear regression approach is used for the analysis of the results, described in the literature as the long term uncertainty in measurement method. The present study clearly indicates the advantages of using proficiency test results in identifying possible constant or proportional bias effects as well as the possibility to compare the laboratory performance with the performance of peer laboratories.

     

Measurement of (90)Sr in environmental samples by cation-exchange and liquid scintillation counting

A new method for the measurement of (90)Sr in environmental samples by cation-exchange and liquid scintillation counting is described. Strontium carbonate is purified by precipitation and ion-exchange, weighed for the determination of chemical yield, dissolved in hydrochloric acid and mixed with the liquid scintillator, Aquasol-2. Two channels of a low-background liquid scintillation counter are used to determine (90)Sr, (90)Y and (89)Sr, free from the effects of environmental tritium. The values of (90)Sr obtained by this method are in good agreement with those from ordinary (90)Y milking and the gas proportional counting method. The concentration of (90)Sr in the air at Tokai-mura in Japan has been measured by the new method.     

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.     

Kinetic spectrophotometric determination of Fe(II) in the presence of Fe(III) by H-point standard addition method in mixed micellar medium

The H-point standard addition method was applied to kinetic data for simultaneous determination of Fe(II) and Fe(III) or selective determination of Fe(II) in the presence of Fe(III). The method is based on the difference in the rate of complex formation between iron in two different oxidation states and methylthymol blue (MTB) at pH 3.5 in mixed cetyltrimethylammonium bromide (CTAB) and Triton X-100 micellar medium. Fe(II) can be determined in the range 0.25-2.5 microg ml(-1) with satisfactory accuracy and precision in the presence of excess Fe(III) and other metal ions that rapidly form complexes with MTB under working condition. The proposed method was successfully applied to the simultaneous determination of Fe(II) and Fe(III) or selective determination of Fe(II) in the presence of Fe(III) in spiked real environmental and synthetic samples with complex composition.     

A semi-automatic combustion method for the simultaneous determination of3H and35S in doubly labelled organic materials by liquid scintillation counting

A sample preparation method developed for the simultaneous liquid scintillation assay of tritium and³⁵S in doubly labelled organic materials is described. The sample is burnt in a stream of oxygen and the radioactive isotope carriers formed are collected separately for individual counting.³⁵S content of the sample is measured as a dilute sulfuric acid solution, while the tritium is counted as water. The procedure is free of cross-contamination and memory effect, provides quantitative analytical recovery, and the final solutions ready for counting are obtained in twelve minutes.     

The determination of241Pu by liquid scintillation spectrometry using the Packard 2250CA

The results of this study indicate that in terms of efficiency, the Packard 2250Ca liquid scintillation spectrometer is sensitive to the scintillation cocktail employed for²⁴¹Pu analysis, particularly when the burst counting circuit is enabled. Cocktails exhibiting low t-SIE values should be avoided since quenching has a critical influence on such a low energy ^– emitter. This effect would be independent of burst circuitry use. Cocktails which include naphthalene type derivatives such as the alkylnaphthalene solvent employed in Optiphase HiSafe 3 and Ultima Gold should be avoided since the broad pulse shapes produced are incompatible with the burst counting circuit which distinguishes background events from true ^– events by means of pulse shape/duration analysis. Efficiency is also sensitive to the concentration of bis-MSB employed in conjunction with the primary fluor. Enhancements in efficiency are observed with appropriate concentrations. These results are in line with previous work with¹⁴C and are postulated as being a consequence of sharpening prompt pulse widths or suppression of afterpulsing. It is recommended that Instafluor should be used to maximize response, or a cocktail such as butyl-PBD/bis-MSB in pseudocumene at rates of 6 and 1.5 mg ml^–1, respectively, where a lower vapor pressure solvent is particularly required.     

Sequential injection spectrophotometric determination of iron as Fe(II) in multi-vitamin preparations using 1,10-phenanthroline as complexing agent

A sequential injection analysis (SIA) system is proposed for the determination of iron (II). Fe(II) was determined by SIA based on the reaction between 1,10-phenanthroline and iron (II), yielding an orange–red colour complex with absorption maximum at 512 nm. The method involved aspiration of 187 μl sample/standard zone followed by a zone of a reagent solution containing 140 μl of 7.8 × 10⁻⁴ mol l⁻¹ 1,10-phenanthroline into a carrier stream to be stacked inside a holding coil and flow reversed through a reaction coil to a detector. The optimum condition was evaluated and the calibration curve is linear over a range of 0.25 to 5.0 mg l⁻¹ of Fe(II) with detection limit of 18 μg l⁻¹. A sample throughput of 40 h⁻¹ was established. This technique is found to be simple, accurate, reproducible and sensitive. The proposed method was successfully applied for the determination of total iron as Fe(II) in pharmaceutical products (multi-vitamin tablets) and is especially useful for the determination of iron (II) in tablets with lower iron (II) contents. The results were found to be in good agreement with the results obtained by manual UV/Vis spectrophotometry and flame atomic absorption spectrometry (FAAS) and with claimed values by the manufacturers.     

A new method for the determination of radon in soil air by the “open vial” and integral counting with a liquid scintillation counter

A new method is described for the determination of Rn in soil gas. Open vials containing a liquid scintillator solution, suspended in a hole of the ground surface, absorb a fixed proportion of Rn present in soil gas. This allows the total Rn concentration to be determined. The method described is rapid, simple and reproducible. It should have many kinds of field application.     

Increasing the sensitivity of241Pu determination for emission and immission control of nuclear installations by aid of liquid scintillation counting

A radiochemical procedure was developed and optimized which allows sensitive²⁴¹Pu measurement in various sample materials. As a first step, Pu isotopes are separated from matrix elements, purified radiochemically, electroplated, and measured by -spectrometry. The electrodeposited Pu is then redissolved in nitric acid and extracted with trioctylphosphinic oxide/cyclohexane. The organic phase is mixed with scintillator cocktail (PPO/Xylene) and Pu is measured with a liquid scintillation counter. The detection limit of the optimized procedure for a counting time of 100 minutes is 50 mBq²⁴¹Pu per sample at a 95% confidence level.     

A new method for simultaneous determination of 226Ra and uranium in aqueous samples by liquid scintillation using chemometrics

In this work, simultaneous determination of low levels of ²²⁶Ra and uranium in aqueous samples were performed by alpha-liquid scintillation counting (LSC) in conjunction with artificial neural network (ANN) and partial least squares (PLS). The counting rates at 73 channels, which were selected by genetic algorithm, were used for training. A PLS model with four latent variables and a principle component ANN model (4-4-2) with linear transfer function after hidden and output layers were created. Total relative error of prediction for PLS and ANN in synthetic mixtures was 18.05% and 24.78%, respectively. The matrix effect was studied by spiking the real samples with radium and uranium. Laser induced fluorescence was used for assessment of uranium prediction results in real samples.