Substoichiometric determination of silver by Neutron Activation Analysis

A rapid and selective method has been developed for the determination of Ag in biological samples and mineral ores by thermal neutron activation analysis employing substoichiometric extraction with 1,2,3-benzotriazole /1,2,3-BT/ into chloroform. The time required for the radiochemical purification and counting of two samples was 1 h. 4.84 g Ag can be determined with an accuracy of 7.44% and a precision of 3.57%.     

Determination of aluminium-26 using a low-level liquid scintillation spectrometer.

The lack of a suitable tracer has severely limited the use of radioisotope tracer experiments in environmental and biological studies on aluminium. The only aluminium radioisotope with a half-life greater than 10 min is the long-lived positron emitter 26Al (t1/2 7.2 x 10(5) years). The exposure of this nuclide and the difficulty in attaining sufficiently low determination limits with standard radioanalytical techniques have restricted its application as a radioactive tracer. The development of a simple method for the routine determination of 26Al using Cerenkov counting and a Quantalus 1220 low-level liquid scintillation spectrometer is reported. For a 300 min counting time, determination limits of about 60 mBq in water samples and 120 mBq in biological (fish gill) samples can be attained. With these levels of determination, the use of 26Al as a tracer is a viable technique for the study of aluminium in environmental and biological systems.     

Rapid pretreatment of environmental samples of food and related materials by a microwave dehydration method

A rapid and simple radioactivity determination method has been developed for food and related environmental samples of a radioactivity level corresponding to 5 mrem/y, Japan AEC's guideline, by pretreating with a modified microwave dehydration apparatus followed by radiation counting. An equation to estimate the heating conditions by the apparatus has been derived, and results calculated by the equation are in good agreement with experimental data. It took less than 4.5 hours to dehydrate by the propossed method, and radiation counting could be started on the day of sampling and dehydration procedure. The lower limit of detection for each radionuclide by the proposed method, using a Ge(Li) detector of 20% relative efficiency, is lower than one half of the needed detection limit to determine and evaluate the 5 mrem/y level. Radionuclide levels in food samples such as vegetables and crustaceans were determined by the proposed method and it was found that they were below the lower dection limit of the proposed method except natural radionuclide⁴⁰K and fallout-originated¹³⁷Cs.     

Simultaneous neutron activation determination of alumina and silica in geological samples using a 5 Ci Pu-Be source

A neutron activation method of analysis for the determination of alumina and silica in geological samples has been developed and applied to some geological standards. Samples of about 4 g /in Cd shield/ were irradiated in the immediate vicinity of a 5 Ci Pu–Be source. Gamma spectra were acquired using a 7.5 cm × 7.5 cm NaI/Tl/ detector. The irradiate-transfer-count sequence was repeated five times in succession, counts being taken cumulatively. Recycling of the sample produced improved counting statistics and better reproducibility.     

Determination of rare earths in low grade uranium ores and SRM-rock by instrumental neutron activation analysis

An instrumental neutron activation analysis technique has been developed for simultaneous determination of 10 REE in low grade U/Zr ores and other geological materials. The samples were irradiated with reactor neutrons for 2 min to 8 hrs followed by a cooling of 30 min to 3 weeks. The γ-ray activity was measured with a semi-planar Ge(Li) detector. A precision of 5% has been obtained by the repeated analysis of NBS-SRM. The technique is relatively simple and adaptable on the routine basis.     

Substoichiometric determination of gold by neutron activation analysis

A rapid method has been developed for the determination of gold in catalyst samples by thermal neutron-activation analysis incorporating substoichiometric solvent extraction of Au/III/ with 1,2,3-benzotriazole /1,2,3-BT/ into n-butanol. The time required for radiochemical purification and counting of two samples and a standard was 1 h.     

Substoichiometric determination of copper by neutron-activation analysis

A rapid and selective method has been developed for the determination of Cu in complex matrices by thermal neutron-activation analysis employing substoichiometric extraction with 1,2,3-benzotriazole /1,2,3-BT/ into chloroform. The time required for radiochemical purification and counting of two samples was 2 h. 1.015 g Cu can be determined with an accuracy of 6.40% and a purification of 5.26%.     

Determination of Fe and Zn in biological samples by radiochemical neutron activation analysis

Radiochemical NAA methods have been developed for the simultaneous determination of Fe and Zn in biological samples. The method involves reactor irradiation, dissolution in 3M HCl and solvent extraction followed by counting on a scintillation gamma-ray spectrometer. Iron was separated with aqueous cupferron and extracted into chloroform while Zn was extracted with 2-thenoyl trifluoroacetone (TTA) into methyl isobutyl ketone (MIBK). Reaction conditions such as pH and the effect of solvents and various ions were studied using tracer activities. The methods have been employed for trace level determination of Fe and Zn in NBS, SRMs, Bowen's Kale, IAEA CRMs and other plant leaves.     

Voltammetric determination of platinum in inorganic complexes and in water, geological and biological matrices using laboratory- and field-based instrumentation

The extremely sensitive catalytic hydrogen ion reduction wave observed after the formation of a platinum-formazone complex at a mercury electrode in a hydrazine-formaldehyde-H2SO4 medium has been utilised to determine platinum voltammetrically in well characterised platinum inorganic complexes (oxidation states O, II and IV) and in biological, geological and water samples. Experimental conditions have been optimised and sample-treatment procedures for various matrices have been critically evaluated for the quantification of platinum by the standard additions method. The determination of platinum in geological samples by this method has been compared with an inductively coupled plasma mass spectrometric method. Both conventional and portable field-based instrumentation have been used in the studies, and the possibility of developing a field-based method for the determination of platinum has been investigated. Despite the inherent sensitivity of the method, which enables concentrations down to 0.01 p.p.b. to be detected in simple matrices, natural levels in water and biological materials, where matrix effects suppress the voltammetric response, are often below the detection limit.     

Substoichiometric determination of Hg by radiochemical neutron activation analysis

A rapid method has been developed for the determination of mercury in environmental samples by thermal neutron activation analysis. Radiochemical separation involves the extraction of Hg/II/ with substoichiometric amounts of 2-mercaptobenzothiazole /2-HMBT/ into chloroform¹. The time required for radiochemical purification and counting of two samples and a standard is about 2 h. Water, sludge and IAEA standard samples were analyzed for Hg concentration by this method.     

Determination of227Ac in geological materials through neutron activation and alpha-spectrometric assay of induced228Th

A new route has been developed for the micro-determination of²²⁷Ac in geological materials by neutron activation. The method is based on intense neutron irradiation of the analysed samples followed by separation and α-spectrometric determination of²²⁸Th, the β-decay product of the 6.1 hrs²²⁸Ac isotope formed. Two alternatives are considered for analysis related to the origin of the analysed matrix. The high sensitivity of the method is documented by the determination of 10^?17 g²²⁷Ac/g sample. The method is successfully applied for age determination of five uranium containing materials and old uranium glass from Bohemia, CSSR.     

Determination of palladium in different samples by neutron activation after selective preconcentration with α-benzildioxime

A procedure is described for the determination of submicrogram quantities of palladium in sea water, biological and geological materials. Palladium is preconcentrated by coprecipitation with α-benzildioxime at pH 2 in the presence of citric acid followed by neutron activation. The method is highly selective and only traces of other metals are adsorbed on the surface of the precipitate. The instrumental variant of counting of long-lived ¹⁰⁹Pd (t$\text{1}\text{2}$ = 13.6 h) after 16-h irradiation gives a detection limit of 10 ng. A further decrease of the detection limit to 1 ng can be attained by removal of radioactive impurities (mainly ²⁴Na, ⁵⁶Mn and ⁸²Br) after washing the dichloromethane extract of dissolved precipitate with an aqueous solution of citric acid containing inactive carriers of bromide, manganese and sodium ions. Palladium (¹⁰⁹Pd) is finally measured by a NaI(Tl) well type scintillation detector. The method can be applied to most environmental samples.     

泡沫塑料动态快速分离富集金方法的研究

本文系统研究了泡沫塑料动态快速分离富集金的方法。对泡沫塑料柱的处理方法,再生及主要共存离子干扰的消除等均做了较详细的研究。提出了一种简便,不控速的金分离富集的方法。该法用于分析0.051～3.59g/t四种不同含量的金标样,结果与推荐值吻合,5次分析结果,相对标准偏差<5％,同时,可用泡沫塑料柱当天连续使用分析拿标样,回收率为93％—109％。     

The simple radiochemical determination of 90Sr in environmental solid samples by solvent extraction

Determination of ⁹⁰Sr in environmental solid samples is a challenging task because of the presence of so many other radionuclides in samples of interest. This problem was dealt with by radiochemical separation of strontium followed by yttrium separation and Cerenkov counting of the high-energy ??-particle emissions of ⁹⁰Y in order to quantitate ⁹⁰Sr. In this work, an improved method is described for the determination of ⁹⁰Sr in soil samples, through the separation of the daughter ⁹⁰Y at equilibrium. The procedure is based on the HDEHP solvent extraction in combination with liquid scintillation spectrometry (LSS). A low background Quantulus has been optimized for low level counting of Cerenkov radiation emitted by the hard ??-emitter ⁹⁰Y. The analytical quality of the method has been checked by analyzing IAEA Soil-375 reference materials. The analytical method has also been successfully applied to the determination of ⁹⁰Sr for moss-soil samples in inter-laboratory exercises through IAEA??s ALMERA network. The chemical recovery for ⁹⁰Y extraction ranged from 80 to 85% and the counting efficiency was 73% in the window 25?C400 keV.     

Rapid determination of selenium and tellurium by atomic-absorption spectrophotometry

A rapid method has been developed for the determination of selenium and tellurium in geological and biological samples. It involves acid digestion of the sample with mineral acids, addition of arsenic as a carrier, reduction of arsenic to co-precipitate selenium and tellurium, dissolution of the precipitate in dilute nitric acid and subsequent determination of selenium and tellurium by conventional atomic-absorption spectrophotometry. Selenium and tellurium have been measured on a routine basis, down to 0.1 ppm.     

新型纳米纤维固相萃取柱制备及其用于组织样品中柔红霉素测定研究

研制出一种新型纳米纤维固相萃取柱,并将其用于大鼠心、肝、脾、肺、肾组织及血浆中柔红霉素的净化、浓缩处理,建立了生物样品中柔红霉素的高效液相荧光检测法.以10%(V/V)HClO4为溶剂,对组织样进行匀浆和离心处理,上清液用纳米纤维小柱净化富集,以50 μL含1%(V/V)冰醋酸的甲醇洗脱,进样20μL检测.流动相为甲醇...     

An accurate procedure for the determination of low levels of iridium in standard reference materials by neutron activation analysis

The paper describes a destructive neutron activation procedure especially set up for the determination of low levels of iridium. Only a few steps are required after irradiation, namely sample dissolution, noble metals adsorption on an ion-exchange column, removal of interfering radionuclides and counting. Successively iridium is removed from the column and the chemical yield evaluated. The method has been used for the determination of iridium in a large variety of standard reference materials, including materials of geological, biological and technological origin, with iridium levels ranging from about 0.005 to 18 ng/g. Results, given as the average of three or more independent analyses, and relative standard deviations, are reported and discussed. Average precision is about 8%, and the sensitivity is 0.004 ng.     

Rapid and sensitive high-performance liquid chromatographic method for the analysis of tryptophan, tyrosine and phenylalanine in biological samples.

In order to overcome problems related to the determination of free tryptophan in biological fluids using conventional methods, we have developed an accurate and reliable procedure based on a specific pretreatment of samples followed by a very rapid and sensitive reversed-phase high-performance liquid chromatographic analysis. The pretreatment consists of adding to the samples of a very low amount of 3 M phosphate buffer to maintain pH in the physiological range followed by ultrafiltration. The precision, reproducibility and sensitivity of our method were also evaluated. The recovery of each amino acid was greater than 92%. The use of a microbore column allows the detection of up to 0.2 pmol/microliter of amino acid. The method has been applied to the analysis of samples obtained from 25 normal and 10 phenylketonuric subjects.     

Effect of sample to detector geometry on the accuracy of instrumental neutron activation analysis and implications for the design of a simple automatic sample-changing wheel suitable for the routine counting of low activity geological samples

The effect of small geometric errors in positioning samples in front of gamma detectors during instrumental neutron activation analysis is discussed and it is shown that, for example, a 0.2 mm repositioning discrepancy for a source to detector distance of 10 mm can cause errors in measured activity of as much as 4 per cent. This calculation has been undertaken for a range of sample-detector distances (5–50 mm) in order to emphasise the importance of sample counting geometry on the accuracy of INAA calibrations. Criteria derived from this investigation have been used to design and construct a simple samplechanging wheel suitable for the routine analysis of low activity geological samples. The effect of the choice of sample wheel size on the magnitude of spectral interference between counting and non-counting samples mounted in the wheel has been considered.     

Fast,selective and sensitive methods for the determination of lead-210 in phosphogypsum and phosphate ore

Two methods are presented for a fast, accurate and precise determination of²¹⁰Pb in industrial samples with a calcium-phosphate and-sulphate matrix. One method combinessolid-liquid extraction on a Pb-selective column Sr^*Spec (Eichrom) with gamma-ray spectrometry of²¹⁰Pb and can be applied to samples >10 g for aselective ²¹⁰Pb determination. The yield is determined gravimetrically. The detection limit is 380 mBq for a 24 h counting period. The other method combineschromatography on Sr^*Spec with liquid scintillation counting of²¹⁰Pb for asensitive ²¹⁰Pb determination and can be applied to samples of up to 1 g. The yield is determined on-line by the UV signal of PbEDTA. The detection limit is 70 mBq for a 2 h counting period. Aspects of accuracy, precision, selectivity, sensitivity and the application of both methods to phosphogypsum and phosphate ores are presented.