Measurement of63Ni in highly radioactive Hanford waste by liquid scintillation counting

Characterization of high-activity radioactive waste stored in underground tanks at Hanford requires determining⁶³Ni (100 y). This low-energy -emitter (E_max 67 keV) must be separated with a high degree of radiochemical purity large amounts of other fission and activation products. The method to be discussed involves multiple precipitation steps with several holdback carriers added, followed by precipitations with dimethylglyoxime, ion exchange, and electrodeposition. The⁵⁹Ni activity is determined by low-energy photon spectrometry. The sample is then stripped from the counting disk with HNO₃, converted to the chloride form, and the⁶³Ni -spectrum is measured with high efficiency by liquid scintillation counting.Pacific Northwest Laboratory is operated for the U.S. Department of Energy under Contract DE-AC06-76RLO-1830.     

Optimisation of liquid scintillation counting conditions for rapid tritium determination in aqueous samples

Several studies were carried out to optimise rapid tritium analysis in fresh waters by ultra-low background liquid scintillation. These included the optimisation of (1) sample/scintillant ratio, (2) pulse shape analysis, and (3) pulse-amplitude comparator, and studies concerning (1) the combination scintillant/vial and (2) the effect of chemiluminescence. The proposed method involves the mixing of 8 ml sample with 12 ml scintillation cocktail Ultima Gold AB in Zinsser low diffusion vials. These are stored during one day before counting in order to reduce chemiluminescence. The minimum detectable activity achieved was 2.2 Bq·l⁻¹ for a total counting time of 360 minutes. In order to test the method, tritium was determined in Ebro river samples.     

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.     

Determination of131I in milk using heterogeneous liquid scintillation counting

Possibilities of the method based on both the selective separation of radioiodine from milk using anion-exchange resin as well as the¹³¹I counting in heterogeneous mixture of this anex with a liquid scintillator are presented. For samples of 4 dm³ volumes, the separation and counting efficiencies about 78% and 45% are achieved. Under the same experimental conditions the background rate is about 0.25 CPS /15 CPM/ and the LLD corresponds to about 7 mBq.dm^–3 /0.2 pCi. dm^–3/.     

Alpha-radiometry of seawater by liquid scintillation counting

Summary Liquid scintillation counting of the alpha-radionuclides after pre-concentration by cation-exchange represents a simple and robust method for the determination of total alpha-radioactivity in seawater. The total efficiency and the minimum detectable activity were calculated to be 95% and 30 mBq, respectively, for a liter sample and 1000-minute measuring time. The method has been applied successfully for the determination of alpha-radioactivity in seawater from five different coastal areas in Cyprus. The average alpha-radioactivity and uranium concentration were found to be 124±8 mBq ^. l^-1 and 3.2±0.2 mg ^. l^-1, respectively.     

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.     

Radon surveys with charcoal and liquid scintillation counting

A detection system for indoor radon using vials with activated charcoal adsorbant and liquid scintillation spectrometry for measurement has been tested thoroughly for months during different seasons. Deviation in the results of two days of exposure from the mean value were at most about ±30%. This system was chosen for a pilot project for large area surveillance in Mühlviertel, a granitic area in the federal state of upper Austria. The distribution system of the detectors is described. The measurement of more than 1200 vials within about two weeks was possible by using ultra low-level liquid scintillation counters (Quantulus). The highest value observed so far was 3150 Bq/m³. Comparing the ratios of the results from the three different measurement systems (charcoal, track etch, electret) significant but acceptable differences were found not only between track etch (3 months exposure) and activated charcoal (3 days exposure), but also between track etch and electret, which both had been exposed for three months. The data are discussed regarding the dose to the population.Note: This paper reflects the personal opinions of the authors.     

A container adsorption study of cadmium using109Cd spiking and liquid scintillation counting

¹⁰⁹Cd may be used as a radiolabel in tracer studies of Cd(II) because of the ease and efficiency with which it may be counted by liquid scintillation counting. It has been found that ppm solutions of Cd²⁺, spiked with¹⁰⁹Cd, may be stored for at least 200 d, in either amber glass or polypropylene containers, without measurable container adsorption, at pH's of 5 or less. At pH's above 5, there is some evidence of container adsorption, particularly in the case of polypropylene containers. Amber glass is recommended if pH's between 5 and 7 must be used for storage.     

Determination of 36Cl in biological shield concrete using pyrohydrolysis and liquid scintillation counting

A method for the determination of 36Cl in biological shield concrete of nuclear reactors was developed. Cl in the concrete sample was extracted quantitatively by pyrohydrolysis at 900 degrees C and recovered in Na2CO3 solution for subsequent measurement of 36Cl by liquid scintillation counting. WO3 was used as an accelerator in the pyrohydrolysis. The Cl extraction procedure was optimized by investigating experimental conditions with the use of ion chromatography and its recovery was evaluated by the analysis of the geochemical reference samples. The detection limit of 36Cl was 0.02 Bq g(-1) for a sample weight of 2 g. The relative standard deviation was 3-7% for the samples containing 0.5 Bq g(-1) levels of 36Cl. The method was applied to determine 36Cl in biological shield concrete of the Japan Power Demonstration Reactor.     

Recent progress and application of low level liquid scintillation counting

The use of an ultra low level liquid scintillation counter with extremely low background, MCA technique, storage and software evaluation of pulse height spectra has given very low LLD's, the possibility of - and -spectrometry to some extent and time saving optimization of counting conditions. Quick and very simple but yet accurate analytical methods could be worked out worked out for environmental measurements: Environmental levels of tritium,¹⁴C in several assimilation products,²²²Rn and²²⁶Ra in water without any sample pretreatment. Suggestions for possible further applications in environmenial monitoring and low level counting are given.     

Rapid determination of 90Sr/90Y in water samples by liquid scintillation and Cherenkov counting

Strontium-90 (⁹⁰Sr) is a ubiquitous contaminant at nuclear facilities, found at high concentrations in spent nuclear fuel and radioactive waste. Due to its long half-life and ability to be transported in groundwater, an accurate method for measuring ⁹⁰Sr in water samples is critical to the monitoring program of any nuclear facility. To address this need, a rapid procedure for sequential separation of Sr/Y was developed and tested in groundwater samples collected from an area of riverbed affected by a ⁹⁰Sr groundwater plume. Sixteen samples, plus spike and water blanks, were analyzed. Five different measurements were performed to determine the ⁹⁰Sr and yttrium-90 (⁹⁰Y) activities in the samples: direct triple-to-double-coincidence ratio (TDCR) Cherenkov counting of ⁹⁰Y, liquid scintillation (LS) counting for ⁹⁰Sr following radiochemical separation, LS counting for ⁹⁰Y following radiochemical separation, Cherenkov counting for ⁹⁰Y following radiochemical separation and LS counting of the Sr samples for ⁹⁰Y in-growth. The counting was done using a low-level Hidex 300SL TDCR counter. Each measurement method was compared for accuracy, sensitivity and efficiency. The results following Cherenkov counting and radiochemical separation were in very good agreement with one another.     

Rapid determination of 226Ra in drinking water samples using dispersive liquid-liquid microextraction coupled with liquid scintillation counting

A new radioanalytical method was developed for rapid determination of ²²⁶Ra in drinking water samples. The method is based on extraction and preconcentration of ²²⁶Ra from a water sample to an organic solvent using a dispersive liquid-liquid microextraction (DLLME) technique followed by radiometric measurement using liquid scintillation counting. In DLLME for ²²⁶Ra, a mixture of an organic extractant (toluene doped with dibenzo-21-crown-7 and 2-theonyltrifluoroacetone) and a disperser solvent (acetonitrile) is rapidly injected into the water sample resulting in the formation of an emulsion. Within the emulsion, ²²⁶Ra reacts with dibenzo-21-crown-7 and 2-theonyltrifluoroacetone and partitions into the fine droplets of toluene. The water/toluene phases were separated by addition of acetonitrile as a de-emulsifier solvent. The toluene phase containing ²²⁶Ra was then measured by liquid scintillation counting. Several parameters were studied to optimize the extraction efficiency of ²²⁶Ra, including water immiscible organic solvent, disperser and de-emulsifier solvent type and their volume, chelating ligands for ²²⁶Ra and their concentrations, inorganic salt additive and its concentration, and equilibrium pH. With the optimized DLLME conditions, the accuracy (expressed as relative bias, B _r ) and method repeatability (expressed as relative precision, S _B ) were determined by spiking ²²⁶Ra at the maximum acceptable concentration level (0.5 Bq L⁻¹) according to the Guidelines for Canadian Drinking Water Quality. Accuracy and repeatability were found to be less than −5% (B _r ) and less than 6% (S _B ), respectively, for both tap water and bottled natural spring water samples. The minimum detectable activity and sample turnaround time for determination of ²²⁶Ra was 33 mBq L⁻¹ and less than 3 h, respectively. The DLLME technique is selective for extraction of ²²⁶Ra from its decay progenies.     

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.     

Alpha-beta discrimination liquid scintillation counting for uranium and its daughters

Advances in liquid scintillation counting (LSC) technologies, such as imporved scintillation cocktail formulations and alpha-beta radiation discrimination, make LSC suitable for applications in uranium process chemistry. Ease of use, low cost, and the huge dynamic range of LSC are distinct advantages for analytical support of actinide processing. All uranium isotopes decay primarily with alpha radiation emission. The immediate short-lived daughters of²³⁸U are²³⁴Th and²³⁴Pa. These nuclides are beta emitters having energy bands that overlap the uranium bands in a liquid scintillation spectrum. The resolution of these overlapping bands by alpha-beta radiation discrimination is useful for uranium quantification and purity verification. Protactinium-234 is a high-energy beta emitter that can be further identified and quantified from it's Cherenkov radiation. Energy spectra were collected on the Packard 2500AB liquid scintillator analyzer for uranyl solutions in diisopropylnaphthalene and pseudocumene based scintillator cocktails. Calibration curves were prepared for nitric, hydrochloric, and sulfuric acid media. Base titrations demonstrated the effect of acid quenching on those system. Ion exchange and water soluble polymer extraction studies are readily followed using liquid scintillation methods.     

Simultaneous determination of alpha and beta-emitting nuclides by liquid scintillation counting

The determination of - and -emitting nuclides has been studied with a commercial liquid scintillation counter /Tri-Carb 2200CA/ equipped with Pulse Shape Analysis /PSA/. The results indicated that the efficiency for -emitters is virtually 100% and discrimination for -emitters is more than 99.9%. Liquid scintillation counting with PSA can be used for the determination of - and -emitting nuclides simultaneously.