Determination of iodine in biological samples by resonance neutron activation

A method of iodine determination in biological samples by means of resonance neutron activation is described. This method has made it possible to determine the iodine content of such samples as children's thyroid gland, grass frog's skin, etc.     

Simultaneous determination of iodine and selenium in biological samples by radiochemical neutron activation analysis

Summary Regarding the favourably sensitive nuclear characteristics of iodine and of selenium but the very different half lives of their induced nuclides ¹²⁸I and ⁷⁵Se, a radiochemical neutron activation analysis method for simultaneous determination of these elements in a single sample was developed. It is based on the double irradiation LICSIR technique — Long Irradiation for Se (40h), Cooling (a week or more), Short Irradiation for iodine (1–15 min) with following Radiochemistry. After the second short irradiation, the sample is ignited in an oxygen flask and iodine and selenium are sequentially and selectively extracted as elemental iodine and 5-nitro-2,1,3 benzoselena diazole chelate. With the described method biological samples were analysed and the reliability of the results was checked by the analyses of different standard reference materials. Good agreement with certified values and high radiochemical purity of the spectra show the applicability of the radiochemical separation developed.     

Non-destructive determination of trace amounts of iodine in biological samples by epithermal neutron activation and Compton suppression gamma-ray spectrometry

In order to investigate the ingestion of iodine by human body and to know its content in organs, instrumental epithermal neutron activation analysis was used in conjunction with Compton suppression gamma-ray spectrometry by measuring the ¹²⁸I short-lived nuclide. The interferences of ²⁴Na and ³⁸Cl induced from NaCl in a sample were reduced by factors of about 6 and 15 to 41 by employing the epithermal neutron activation and Compton suppression gamma-ray spectrometry, respectively. The present method can be used to determine iodine at levels higher than 11 ppb. It was applied to the determination of iodine of more than 35 ppb in various biological reference materials.     

Determination of iodine in biological materials by neutron activation analysis

A method of determination of iodine (total and PBI) in serum, urine and other biological materials has been developed. The method consists in a gamma-spectrometric measurement of¹²⁸I activity after its radiochemical separation. The radiochemical separation procedure includes wet decomposition of the samples in a nitric acid medium followed by a few separation steps, the essential step being the substoichiometric extraction of iodide with a chloroform solution of tetraphenylarsonium chloride. Owing to the application of the substoichiometric separation, a high radiochemical purity of the separated iodine is achieved and the determination of the yield of radiochemical separation is not necessary.     

Dithiocarbamate extraction of trace amounts of selenium from biological samples for neutron activation analysis

A three-step method has been developed for extracting trace amounts of selenium from biological samples for neutron activation analysis /NAA/. After acid digestion, the sample is first extracted with lead diethyldithiocarbamate at pH 4 to remove a number of interfering elements. Next, selenium is extracted with sodium diethyldithiocarbamate into chloroform at pH 1.5. Finally, selenium is back-extracted with concentrated nitric acid for NAA. Analysis of selenium extracted from four standard reference materials resulted in excellent agreement with the certified values of selenium concentration. A detection limit of 0.05 g has been achieved.     

Determining trace amounts of nickel in plant samples by neutron activation analysis

Neutron activation analysis of plant samples for trace amounts of nickel has applications in various fields. Landsberger and Robinson (Trans Am Nucl Soc 102:187–188, 2010) found their measurement of the concentrations of nickel for different NIST reference materials to be significantly greater than the certified values when measuring nickel from the 810.8 keV gamma ray that comes from ⁵⁸Co from the ⁵⁸Ni(n,p) reaction. They determined that this overestimation was due to a significant interference by the presence of ¹⁵²Eu at 810.5 keV, and presented a method for correcting this interference. Their method involved a long thermal irradiation and correction of gamma ray counts based on the 1,408 keV belonging to ¹⁵²Eu. This paper presents an alternative approach, which involves irradiating the samples with epithermal neutrons, which suppressed the ¹⁵²Eu to the point of being negligible for samples with low levels of europium. Both methods were determined to work well for the identification of nickel concentrations by neutron activation analysis.     

Estimates of iodine in biological materials by epithermal neutron activation analysis

Iodine abundances in NBS biological SRMs and various organs of rats were evaluated by epithermal neutron activation analysis with a boron carbide filter. Detectability of iodine in different biological materials by this method is discussed.

     

Determination of picogram amounts of technetium in environmental samples by neutron activation analysis

A procedure for the determination of trace amounts of ⁹⁹Tc in filter paper and vegetation samples by neutron activation analysis has been developed. The procedure consists of the following major steps: (a) pre-irradiation separation of technetium from the sample and purification of the technetium fraction; (b) thermal neutron irradiation of the ⁹⁹Tc fraction to produce ¹⁰⁰Tc ; (c) post-irradiation separation and purification of ¹⁰⁰Tc from other activated nuclides: (d) counting of the 16-sec ¹⁰⁰Tc in a low-background β-counter.

The estimated detection limits for ⁹⁹Tc by this procedure with irradiations at a thermal neutron flux of about 5.10¹³ n cm^-2 sec^-1 are: 5.lO^-12g ⁹⁹Tc in filter paper samples, and 9. 10^-12 g ⁹⁹Tc in vegetation samples.     

Determination of Hg in biological samples by substoichiometric neutron activation analysis

The method described here involves the irradiation of biological samples and a g quantity of standard with thermal neutrons at the self-serve position in the CIRUS reactor, followed by dissolution of the sample and standard in the presence of milligram amounts of carrier. Both the sample and the standard are subjected to substoichiometric extraction under controlled experimental conditions with ethyl thioacetoacetate into chloroform. An aliquot of the organic phase is counted on a -spectrometer. The concentration of Hg in various biological samples and the accuracy, precision, and sensitivity of the method are discussed.     

Determination of copper in biological samples by substoichiometric neutron activation analysis

A method has been described for the determination of trace amounts of copper in biological samples by thermal neutron activation analysis, involving radiochemical separation of copper from irradiated matrix employing substoichiometric extraction of Cu/II/ with 2-mercaptobenzothiazole /2-HMBT/ into chloroform. 4.01 g of Cu/II/ can be determined with an accuracy of 3.13% and precision of 1.08%.     

Simultaneous radiochemical neutron activation analysis of iodine, uranium and mercury in biological and environmental samples

The determination of medium and long-lived nuclides can be combined with short-lived ones if a medium or long irradiation is made prior to the short irradiation and radiochemical processing. Thus, an RNAA method previously developed for determination of iodine based on the reaction¹²⁷I(n,)¹²⁸I (T _1/2=25 m) using oxygen flask ignition of the irradiated sample, followed by solvent extraction with an iodine-iodide redox cycle, was combined with an overnight preirradiation to induce the²³⁵U fission product¹³³I (T _1/2=20.8 h). By reactivating the sample, cooled 1–2 days after the first irradiation, for few minutes both¹²⁸I and¹³³I could be quantified in the separated iodine fraction. Non-combustible inorganic materials (e.g., sediment, soil, etc.) can be successfully ignited after mixing with excess cellulose powder. Chemical yields for iodine were determined spectrophotometrically in the organic phase, while homogeneously spiked Whatman cellulose powder was used as uranium standard. Mercury is also released on ignition and collected in the absorbing solution, from where it was separated by toluene extraction. Its chemical yield was determined for each aliquot using²⁰³Hg tracer and counting on an LEPD. Results for some suitable SRMs are presented, and the general features of the double irradiation technique discussed.     

Determination of trace amounts of copper and selenium in biological samples by chemical separation prior to neutron activation analysis

It was found that Cu and Se can be relatively easily and accurately determined by preconcentration of Cu and Se prior to the determination by neutron activation analysis with the short-lived IRN's (Indicator Radionuclides)⁶⁶Cu and^77mSe. The method consists of wet acid digestion followed by coprecipitation with lead tetramethylenedithiocarbamate. The precipitate was collected, irradiated and counted. The validity of the method was confirmed both by internal checks, as the measurement also by⁷⁵Se and by the use of two reference material of biological origin. The limit of detection was found to be 20 ng Se and 50 ng Cu for a 0.1 g sample.     

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.     

Epithermal instrumental neutron activation analysis of biological reference materials for iodine

Epithermal instrumental neutron activation analysis (EINAA) methods have been optimized and applied to several biological reference materials and selected food items for the determination of iodine. The method involves irradiation of the samples for different periods in epi-cadmium and/or epi-boron flux of the Dalhousie University SLOWPOKE-2 reactor and direct counting without any pre-treatment on a 25-cm³ hyperpure Ge detector. The 443 keV photopeak of ¹²⁸I is used for assaying the iodine content. Precision of measurements, expressed as the relative standard deviation, is 10–15% at 200–500 ppb and 3–12% at 500–6000 ppb levels of iodine. Accuracy of iodine measurements is within 5%. The detection limits for iodine in several biological materials with cadmium and boron, either alone or a combination of the two, as thermal neutron shields have been found to vary between 0.1 and 0.4 mg · kg^–1 for different periods of irradiation, decay and counting. The results suggest that the EINAA methods can be successfully applied to biological materials for routine analysis of iodine at levels higher than 200 ppb.     

Determination of chlorine, bromine and iodine in rock samples by radiochemical neutron activation analysis

Chlorine, bromine and iodine (hereafter, halogens) were detemined for rock samples by radiochemical neutron activation analysis. The powdered samples and reference standards prepared from chemical reagents were simultaneously irradiated for 10 to 30 minutes with or without a cadmium filter in a TRIGA-II reactor at the Institute for Atomic Energy, Rikkyo University. The samples were subjected to radiochemical procedures of halogens immediately after the irradiation. Iodine was firstly precipitated as PdI₂, and chlorine and bromine were successively precipitated as Ag-halides at the same time. In this study, geological standard rocks, sedimentary rocks and meteorites were analyzed for trace halogens. In some Antarctic meteorites, iodine contents were observed to be anomalously high. Chlorine contents also are somewhat high. The overabundance of iodine and chlorine must be caused by terrestrial contamination on the Antarctica.     

Determination of thallium in biological samples by thermal neutron activation analysis and low-level beta-counting

A procedure is described for the determination of thallium in complex biological matrices by thermal neutron activation analysis employing substoichiometric extraction of thallium(I) with 2-mercaptobenzothiazole (2-HMBT) at a pH of 7.5 into chloroform, and low-level beta-counting.     

Determination of trace level mercury in biological and environmental samples by neutron activation analysis

Sorptivity studies with Chelex 100 column indicated chloride to be the best medium for the sorption of mercury. A radiochemical separation procedure has been developed for the determination of mercury by neutron activation analysis utilizing sorption of mercury on Chelex 100. The method was checked with Orchard Leaves and Tuna Fish standards from the National Institute of Standards and Technology.     

Determination of isotopic thorium in biological samples by combined alpha-spectrometry and neutron activation analysis

The determination of isotopic thorium by alpha-spectrometric methods is a routine practice for bioassay and environmental measurement programs. Alpha-spectrometry has excellent detection limits (by mass) for all isotopes of thorium except²³²Th due to its extremely long half-life. This paper reports a pre-concentration neutron activation analysis (PCNAA) method for²³²Th that may be performed following alpha-spectrometry if a suitable source preparation material is utilized. Human tissues and other samples were spiked with²²⁹Th and the thorium was isolated from the sample using ion exchange chromatography. The thorium was then electrodeposited from a sulfate-based medium onto a vanadium planchet, counted by alpha-spectrometry, and then analyzed for²³²Th by neutron activation analysis. The radiochemical yield was determined from the alpha-spectrometric method. Detection limits for²³²Th by this PCNAA method are approximately 50 times lower than achieved by alphaspectrometry.     

Determination of trace iodine in rock samples by epiterhmal neutron activation analysis involving rapid radiochemical separation

Applying rapid radiochemical separation of iodine coupled with epithermal neutron activation, we reliably determined trace amounts /6–95 ng/ of iodine in rock samples such as sedimentary rocks and chondritic meteorites. Our data on meteorites are in good agreement with literature values, but for sedimentary rocks the present data were systematically lower than the literature values. Based on the data from duplicate analyses of some sedimentary rocks and the results of tracer experiments employed parallel to the rock analyses, we concluded that the analytical results obtained in this work for sedimentary rocks were more reliable than the literature values.