Radiochemical separation of rhenium with crown ether for neutron activation analysis in rocks

The extraction behavior of perrhenate with crown ethers has been studied and methods for the separation and determination of rhenium have been developed. Perrhenate anion can be quantitatively extracted into nitrobenzene by benzo-15-crown-5 (B15C5) from 2M potassium hydroxide and back-extracted by sodium phosphate buffer solution. The molar ratio of B15C5 to KReO₄ in the extracted species is probably 21. Rhenium was satisfactorily determined by neutron activation method in rock samples.     

Extraction of uranium with crown ether carboxylic acids for neutron activation analysis

Uranium in aqueous solution can be extracted by sym-dibenzo-16-crown-5-oxy-acetic acid and its modified analogue 2-/sym-dibenzo-16-crown-5-oxy/-hexanoic acid into chloroform in the pH range 5.5–6.0. The extraction method combined with neutron activation analysis provides a sensitive method for the determination of uranium in natural waters.     

Solvent extraction separation of rubidium with dicyclohexano-18-crown-6

Rubidium is extracted quantitatively at pH 3.0-7.0 by 0.01M dicyclohexano-18-crown-6 in methylene chloride from 0.01M picric acid, stripped with 2M nitric acid and determined by flame photometry or atomic-absorption spectrometry. It can be separated from the most alkali and alkaline-earth metals, but the tolerance levels for potassium, ammonium and barium are rather low. The common anions, including those of some organic acids, are tolerated in fairly high amounts. The method has been applied to analysis of chloride schist rock and lepidolite for rubidium. The analysis takes an hour.     

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.     

Rapid determination of dysprosium in rock samples by neutron activation analysis with a ge(li) detector after chemical separation

A neutron activation method for the rapid determination of dysprosium in rocks, based on simple chemical separation and γ-spectrometry with a lithiumdrifted germanium detector, is described. The 94.7-keV photopeak of dysprosium-165 (2.3 h half-life) was measured. Several geochemical standard rocks covering a variety of rock types were analyzed. The detection limit was 0.005 μg of dysprosium. A precision of ±4.7% was obtained on 7 separate analyses of a basalt standard rock. The accuracy of the method is discussed.     

Determination of rare-earth eleemnts in rock samples by neutron activation analysis

A Ge(Li) detector combined with cation exchange separation has been used for the determination of 12 rare-earth elements (La, Ce, Nd, Sm, Eu, Gd, Tb, Ho, Er, Tm, Yb, and Lu) in rock samples by neutron activation analysis. After purification by the conventional hydroxide-fluoride precipitation, the rare-earth elements are separated into two fractions, light (La-Tb) and heavy (Ho-Lu), by EDTA cation exchange, and the γ-activities of the two fractions are measured by a Ge(Li) detector. The heavy rare-earths, such as Ho, Er, and Tm, can be easily γ-counted without serious interference from the intense Compton background and photopeaks due to the light rare-earths such as¹⁴⁰La,¹⁵³Sm,¹⁵²Eu, and¹⁶⁰Tb. The chemical yields (60%) for the individual rare-earths are determined by a reactivation technique. The results obtained for the U.S. Geological Survey standard rocks G-1 and W-1 are compared with the previously reported data.     

Determination of Sc in rock samples by substoichiometric thermal neutron activation analysis

A rapid, selective and simple method has been developed for the determination of Sc in rock samples by thermal neutron activation analysis, employing substoichiometric solvent extraction of Sc(III) with alizarin into 1-octanol. Two samples and a standard can be processed and counted within three hours.     

Solvent extraction separation of gallium with 18crown6 from chloride media

Gallium was quantitatively extracted with 0.02M 18crown6 in methylene chloride from 6M hydrochloric acid, then stripped with 1M acetic acid and determined with 2-(pyridylazo)naphthol with measurement at 545 nm. Gallium was separated from indium, thallium, lead, aluminium and bismuth. The method was applied to determination of gallium in bauxite.     

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.     

Determination of iridium and gold in rock samples by using pre-concentration neutron activation analysis

Nickel sulfide (NiS) fire assay was used for the pre-concentration of Ir and Au in rock samples. The beads obtained after fire assay were irradiated directly with neutrons to determine Ir and Au. To suppress the reaction of ⁵⁸Ni(n,p)⁵⁸Co, the fire assay was carried out by using a small amount of Ni (0.0625 g) and the NiS bead samples were irradiated by neutrons with high Cd ratios. Analytical results of Ir and Au for rock samples were close to literature values, confirming that our procedure of INAA with pre-concentration can be applied to rock samples for the determination of ppb to sub-ppb level of Ir and Au.     

Determination of rare-earth elements in rock samples by neutron activation analysis with a lithium-drifted germanium detector after chemical group-separation

A lithium-drifted germanium detector combined with chemical group-separation has been utilized for the determination of rare-earth elements (La, Ce, Nd, Sm, Eu, Gd, Tb, Tm, Yb and Lu) in rock samples by neutron activation. This procedure has the advantage of a low background level which cannot be attained in the non-destructive method. The combination of the Ge(Li) detector and chemical group-separation also offers a distinct simplification in the correction of contributions from other nuclides. For optimum utility of a Ge(Li) detector in neutron activation analysis, chemical group-separations are recommended.     

Substoichiometric isotope-dilution analysis for strontium by liquid-liquid extraction with a macrocyclic crown ether or cryptand

Strontium(II) is substoichiometrically extracted into 1,2-dichloroethane with 1.0 × 10^?4 M cryptand-2.2.2 or 18-crown-6 in the presence of 1.0 ×10.2 M picrate at pH 8–10 or 7–9, respectively. A constant substoichiometric amount of strontium(II) is extracted (relative standard deviation, 0.5%). The method combined with isotope dilution is applied to determine strontium(II) in a seaweed sample (Laminaria religiosa Miyabe); the values obtained were 546 ± 9 μg g^?1 with cryptand-2.2.2 and 546 ± 7 μg g^?1 with 18-crown-6.     

On the separation of molybdenum and technetium crown ether as extraction agent

Separation of⁹⁹Mo and^99mTc can be performed with high selectivity using the crown ether 2,3,11,12-dibenzo-1,4,7,10,13,16-hexaoxacyclooctadeca-2,11-diene /DB18C6/ diluted with nitrobenzene. The high efficiency is attributed to the rather low extractability of molybdenum as compared with that of technetium.     

Estimation of rubidium in coconut palm leaves by neutron activation analysis

A simple and rapid method is described for the estimation of the rubidium in coconut palm leaves by neutron activation analysis. The method is found suitable for the estimation of stable Rb used as a tracer in root distribution studies. The average of five determinations is 5.15 μg, which varies between 5.07 μg and 5.26 μg at 95% confidence limit.     

Feasibility studies of neutron activation analysis with kilogram-size samples

Instrumental neutron activation analysis (INAA) can now directly be applied to samples with masses in the kilogram range. It enables the analysis of material which is considered to be not representative at the scale of the traditional analytical portion, but representative at much larger scale. Large sample INAA (LS-INAA) circumpasses various problems associated with sample-size reduction and homogenization. Examples of feasibility studies are given as on construction waste, contaminated soil, harbour sediment and recyclable material. Also the economics of this method of analysis is discussed. Received: 30 October 1996 / Revised: 3 April 1997 / Accepted: 16 April 1997     

Instrumental neutron activation analysis of Obsidian rock

An instrumental neutron activation analysis technique has been developed for the simultaneous determination of up to 30 elements including major, minor and trace elements in Obsidian Rock (a proposed NBS-SRM-278). INAA method involves both short and long irradiations followed by gamma-ray activity measurement with a Ge(Li) detector. The accuracy of the procedure has been checked by analyzing IAEA Reference Materials.     

Solvent extraction of silver and thallium picrates with poly- and bis-(crown ether)s

Summary Solvent extraction of silver and thallium picrates by new poly- and bis(crown ether)s, which contain benzo-15-crown-5 or benzo-18-crown-6 moieties, was carried out in water-chloroform system. The poly- and bis(crown ether)s showed higher extractability for both metals than the corresponding monocyclic crown ethers.Especially poly- and bis(benzo-15-crown-5) were found to be quite effective extracting agents for Tl⁺.The extraction equilibrium constants and the complexation constants for the chloroform phase were also estimated.

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Lösungsmittelextraktion von Silber- und Thalliumpikraten mit Poly- und Bis-Kronenethern

Zusammenfassung Die Extraktion der Pikrate wurde in Wasser/Chloroform mit neuen Poly- und Bis-Kronenethern durchgeführt, die Benzo-15-Krone-5- oder Benzo-18-krone-6-Komponenten enthielten. Die Poly- und Bis-Kronenether wiesen für beide Metalle eine bessere Extrahierbarkeit auf als die entsprechenden monocyclischen Kronenether. Insbesondere Poly- und Bis(benzo-15-krone-5) erwiesen sich als wirkungsvolle Extraktionsmittel für Thallium(I). Die Extraktions-Gleichgewichtskonstanten und die Komplexbildungskonstanten für die Chloroformphase wurden bestimmt.

     

Solvent extraction of alkaline earth metal picrates with poly- and bis(crown ether)s

Summary Solvent extraction of alkaline earth metal picrates with poly- and bis(crown ether)s containing benzo-15-crown-5- and benzo-18-crown-6 moieties was carried out in a water-chloroform system. The poly- and bis(crown ether)s showed larger extractability for the metal picrates than the corresponding monocyclic crown ethers. Especially, poly- and bis(benzo-15-crown-5), and bis(benzo-18-crown-6) were found to have relatively high extractability and selectivity for Ba²⁺ and Sr²⁺, respectively.

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Lösungsmittelextraktion von Erdalkalipikraten mit Hilfe von Poly- und Bis-Kronenethern

Zusammenfassung Poly- und Bis-Kronenether mit Benzo-15-krone-5- und Benzo-18-krone-6-Einheiten wurden zur Extraktion von Erdalkalipikraten im Wasser-Chloroform-System verwendet. Die genannten Ether zeigten eine bessere Extraktionsfähigkeit für die Pikrate als die entsprechenden monocyclischen Kronenether. Im Falle von Ba²⁺ und Sr²⁺ ergab sich eine besonders gute Extrahierbarkeit und Selektivität mit Poly- und Bis(benzo-15-krone-5)- und Bis(benzo-18-krone-6)-Ethern.