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.     

Simultaneous determination of35S and14C in double-labelled organic compounds by liquid scintillation counting

An isotope analytical method for the simultaneous determination of³⁵S and¹⁴C in double-labelled organic compounds by liquid scintillation counting is described. The sample is burned in a stream of oxygen. Sulfur oxides are converted to sulfuric acid and separated from other combustion products, including carbon-14 dioxide, on a heated quartz wool column previously wetted with hydrogen peroxide. Carbon dioxide is collected from the gas stream by an absorbent suitable for liquid scintillation counting. The residual sulfuric acid is rinsed off the column with water and the aqueous solution obtained is mixed with a liquid scintillation cocktail for radioactivity measurement. The final solutions ready for counting are obtained in less than fifteen minutes, quantitative collection recovery is achieved and no cross contamination occurs.     

Optimization of liquid scintillation counting techniques for the determination of carbon-14 in environmental samples

The goal of this work was to optimize the liquid scintillation counting techniques for the determination of¹⁴C in stack effluent gases and in environmental samples such as biological and air samples. Carbon-14 activities in most environmental samples were measured with the direct CO₂ absorption method. The highest figures of merit were found through the variation of Carbosorb E and Permafluor V ratio, and measurement windows. The best condition was an 1:1 volume ratio. Average 2.35 g of CO₂ was reproducibly absorbed in the 20 ml mixture within 40 minutes. The counting efficiency determined by repeated analysis of NIST oxalic acid standard and the background count rate were measured to be 58.8±1.4% and 1.88±0.06 cpm, respectively, in case of saturated solution. The correction curves of counting efficiency for partially saturated solutions and for saturated solutions with quenching were prepared, respectively. The overall uncertainty of the sample specific activity for near background levels was estimated to be about 7% for 4 hours counting at 95% confidence level. Stack effluent gas samples were measured by a gel suspension counting method. After precipitation of CO₂ in the form of BaCO₃, 140 mg of which was mixed with 6 ml H₂O and 12 ml of Instagel XF. The counting efficiency was measured to be 71.5±1.7% and the typical sensitivity of this technique was about 510 mBq/m³ for a 100 min count at a background count rate of 4.7 cpm. For the benzene counting method measurements were performed with a mixture of 3 ml benzene and 1 ml of scintillation cocktail (5 g of butyl-PBD in 100 ml of scintillation-grade toluene) in a low potassium 7 ml borosilicate glass vial. The counting efficiency and the background count rate were measured to be 64.3±1.0% and 0.51±0.05 cpm, respectively. The long-term stability of samples has been checked for all the counting techniques over a two week period, during which no apparent change in counting efficiency and background level was found.     

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.

     

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.     

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.     

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/.     

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.     

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.     

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.     

Alpha-liquid scintillation counting for the determination of plutonium

Liquid scintillation counting is useful and extensively employed for -activity measurement. However, quenching is observed and erroneous results are obtained when the size of the solution aliquot and its acidity exceed certain limits. A simple procedure has been developed to overcome the quenching effect of volume and acidity on -counting.     

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.     

Application of the double ratio technique to emulsion systems for liquid scintillation counting of3H and14C labelled materials

Emulsion counting, more correctly known as colloid counting, is the most widely practised technique for the radioassay of aqueous sample types by the liquid scintillation technique. The double ratio technique can be used to determine whether or not radioactivity is being counted with true solution efficiency, and was applied to a range of systems consisting of deionised water, Triton X-100 and toluene (containing³H-water,³H-toluene or¹⁴C-toluene). Some hypotheses were developed in an attempt to explain the double ratio values obtained for the various systems studied.     

Simultaneous determination of 152Eu and 241Am in liquid solution by liquid scintillation counting

¹⁵²Eu and ²⁴¹Am are the most frequently used radiotracers in the separation studies on trivalent minor actinides and lanthanides. In almost all those studies, the determination of ¹⁵²Eu and ²⁴¹Am has been based on measuring their γ radiation by using a NaI(Tl) scintillation detector and/or a germanium detector. In this study, based on measuring the β particles and mono-energy electrons from ¹⁵²Eu and the α particles from ²⁴¹Am, we provide a new option to simultaneously determine the radioactivities of ¹⁵²Eu and ²⁴¹Am by liquid scintillation counting (LSC) with the aid of α/β discrimination. If the count rate ratio of ²⁴¹Am to ¹⁵²Eu is within the range of 100:1–1:100, the radioactivities of ¹⁵²Eu and ²⁴¹Am in mixed samples can be simultaneously determined by LSC with the errors less than 5 %. In addition, the interferences of ²⁴¹Am on Eu are divided into two parts: inside and outside the ²⁴¹Am region of interest. Only if the count rate ratio of ²⁴¹Am to Eu is more than 10:1, should the latter interference be in consideration.     

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.     

Radio high-performance liquid chromatographic determination of 14C-labelled LF 2-0254, A 1,4-dihydropyridine calcium antagonist, in rat and dog plasma using off-line liquid scintillation counting

LF 2-0254 is a 1,4-dihydropyridine calcium antagonist with a slow onset of action. The pharmacokinetics of [14C]LF 2-0254 were studied in rats and dogs. A sensitive high-performance liquid chromatographic method using liquid scintillation counting was developed for the quantitation of labelled LF 2-0254 in plasma. The peak height of the internal standard in the chromatogram was measured by UV detection and the mobile phase containing the chromatographic peak of [14C]LF 2-0254 was collected and counted for radioactivity. The concentration of labelled drug in the plasma was then determined using a calibration graph constructed from the determination of [14C]LF 2-0254 of known specific activities. The limit of determination was dependent on the specific activity of the drug administered. This method permits the measurement of the radioactive drug in biological fluids.     

A spectral overlap method for self monitoring quench correction in double isotope liquid scintillation counting

A method for quench correction of samples with double radioactive labelling is described. Each nuclide makes a contribution to the counting rate of three channels of a liquid scintillation counter. This channel overlap is an essential requirement of the calibration procedure rather than a limitation, and allows more freedom in the choice of counting conditions. After calibration with suitable standards the method will tolerate wide variations in the ratio of one isotope to the other extending to single label samples of either isotope. This is the outstanding advantage over the channel ratio method which requires a statistically significant counting rate for the higher energy isotope. The method takes advantage of the facilities offered by a computer which may be on line or remote.¹⁴C and tritium are used to demonstrate the utility of the method.