The distribution of trace elements in normal human liver determined by semi-automated radiochemical neutron activation analysis

The eight segments of five normal human livers are analysed for 25 trace elements by radiochemical NAA. This consits of an automated wet destruction of the samples and two distillations, followed by ion exchange procedures. Ru is used as triple-comparator for the standardisation. Short-lived and matrix-isotopes are standardised by the Bowen's kale powder. The results reveal that the coefficient of variation within the liver is smaller than 10% for the elements Cd, Cl, Cs, Cu, Fe, K, Mg, Mn, Rb, Se and Zn. The highest range observed for the elements As, Br, Co, Cr, Hg, La, Mo, Na and Sb within a liver is smaller than the range observed between the five livers.     

On processing standards in radiochemical neutron activation analysis

In radiochemical neutron activation analysis, standards may be measured directly or subjected to the same radiochemical processing as the sample. Some considerations in regard to processing are examined, and the advantages and disadvantages of this approach discussed. It is concluded that processing of standards is often inadvisable and can lead to errors, particularly if used as a substitute for radiochemical yield determinations.     

Determination of rare-earth elements in steels by radiochemical neutron activation analysis

For the separation of rare-earth elements from steel, with a cation exchange resin, separation experiments were performed on NIST reference materials of SRM-363 and SRM-364. Iron, Na, Cr, Mn, Co, Cu, As, Mo, Sb and W were separated in 2M hydrochloric acid, five rare-earth elements, La, Ce, Pr, Nd and Sm and three other elements, Hf, Zr and Ba were separated using 8M nitric acid. Each element was determined by a single comparator method using two monitors, gold and cobalt.     

Extraction-chromatographic system TBP-HBr in radiochemical neutron activation analysis of high-purity materials

The extraction and extraction-chromatographic behaviour of a variety of elements in the TBP-HBr system with concentrations from 0.1 to 7M HBr has been studied. The results allowed the development of simple procedures for radiochemical neutron activation determination of 22 impurity elements (Na, K, Sc, Cr, Mn, Fe, Co, Ni, Cu, Ga, As, Se, Rb, Sr, Zn, Mo, Ag, Sb, Te, Ba, La, Hf and W) in high-purity cadmium and indium samples with detection limits from 1 g g^–1 for Fe and Zr to 0.01 ng g^–1 for Na, Sc, Mn with relative standard deviations < 0.15. To increase the selectivity of the extraction-chromatographic separation, use was made of extraction suppression and co-extraction effects. The procedure for the extraction-chromatographic separation of scandium from a number of other elements is described as an example. The procedure can be used for simultaneous quantitative separation of impurity radionuclides from radiation produced long-life scandium radionuclides in the neutron activation analysis of titanium and vanadium.     

Determination of individual rare earth elements in Vietnamese monazite by radiochemical neutron activation analysis

Radiochemical neutron activation analysis (RNAA) has been applied for determination of rare earth elements (REE) in Vietnamese monazite. The chemical separation procedure used is based on the chromatographic elution of rare earth groups, after the separation of²³³Pa(Th) in irradiated monazite samples by coprecipitation with MnO₂, the rare earth elements were retained by Biorad AG1×8 resin column in 10% 15.4M HNO₃-90% methanol solution. The elution of heavy rare earth (HREE) and middle rare earth (MREE) groups was carried out with 10% 1M HNO₃-90% methanol and 10% 0.05M HNO₃-90% methanol solution, respectively; while the light rare earths (LREE) were eluted from the column by 0.1M HNO₃ solution. The accuracy of the method was checked by the analysis of granodiorite GSP-I and the rare earth values were in good agreement.     

Distribution patterns of rare-earth elements in biological materials evaluated by radiochemical neutron activation analysis

This study deals with the quantitative determination of eight REE's viz, La, Ce, Nd, Sm, Eu, Tb, Yb, and Lu as an Integral part of a post-irradiation chemical separation scheme for the determination of 14 trace elements in biological materials. REE values are given for NBS Orchard Leaves SRM 1571, NBS Bovine Liver SRM 1577 and Bowen's Kale, as well as for some other biological (reference) materials of plant, animal and human origin. Chondritic-normalized REE patterns of these materials are discussed. It is shown that differentiations in REE-pattern between soil and plant may occur, and also that within the human body different modes of fractionation of REE's take place.     

Determination of cadmium using radiochemical neutron activation analysis

A method has been developed for the determination of cadmium in samples of food and biological materials using neutron activation analysis with radiochemical separation. The irradiated sample is digested in presence of cadmium carrier, with a nitric-perchloric mixture, evaporated to dryness, dissolved in 6M HCl and placed onto an ion exchange column loaded with Dowex 1-X8 resin in chloride form and conditioned with HCl 6M. The cadmium is retained in the resin. After a washing procedure with several portions of HCl of decreasing concentration, the cadmium is eluted with an ammonia-ammonium chloride buffer. The activity of ^115mIn which is in equilibrium with ¹¹⁵Cd, is measured using a NaI(Tl) well type detector. The method has been evaluated by analyzing certified reference materials with cadmium concentrations covering a range of 0.020 to 200 mg^.kg^-1. The agreement of the results with the certified values is within 95%, which gives an indication of the sensitivity and accuracy of the proposed method.     

A group separation scheme for radiochemical neutron activation analysis for 24 trace elements in rocks and minerals

A group separation scheme has been developed for radiochemical neutron activation analysis for Ca, Cu, Zn, Ga, Rb, Sr, Zr, Sb, Cs, Ba, La, Nd, Sm, Eu, Gd, Tb, Ho, Tm, Yb, Lu, Hf, Ta, W and Th in a wide variety of silicate rocks and minerals, especially ultrabasic rocks and mafic minerals. The samples are decomposed in a hydrofluoric acid-nitric acid mixture in a PTFE-lined bomb. The soluble fluorides (Cu, Zn, Ga, Rb, Zr, Sb, Cs, Ht, Ta, W and Pa) are separated into three groups of elements by sequential elution from a cationexchange resin. The insoluble fluorides (Ca, Rb, Sr, Cs, Ba and REE) are dissolved and purified from interfering iron and scandium activities by extraction with tri-n-butyl phosphate. If necessary, the four main groups can be purified further from interfering activities such as ⁵⁹Fe, ⁵¹Cr and ⁶⁰Co. The accuracy and reproducibility of the procedure were tested by repeated analysis of U.S. Geological Survey standard granite G-2, andesite AGV-1 and dunite DTS-1.     

Determination of uranium, thorium, and 20 other elements in high-purity tungsten by radiochemical neutron activation analysis

A radiochemical neutron activation analysis method for the determination of 22 elements in high-purity tungsten has been developed. For the assay of indicator radionuclides with long half-lives, the radiochemical separation was performed from HF/H₂O₂, HF/NH₄F and HCl/H₂SO₄ media by a combination of cation and anion exchange on a Dowex 50 W × 8 and Dowex 1 × 8 column. An effective removal of the matrix-produced radionuclides of W and Re was achieved. U was determined via ¹⁴⁰La, the daughter nuclide of the fission product ¹⁴⁰Ba. Limits of detection of 2 ng/g for U and 0.02 ng/g for Th can be achieved. For the other elements, the limits of detection are between 0.004 ng/g (Sc) and 200 ng/g (Sr). The elements Hf, Ta and Sb could be determined by instrumental neutron activation analysis. This method was applied to the analysis of two tungsten powder samples of different purity grade. The results and limits of detection are compared with those of other methods. Received: 28 July 1997 / Revised: 29 October 1997 / Accepted: 1 November 1997     

Determination of uranium, thorium, and 20 other elements in high-purity tungsten by radiochemical neutron activation analysis

A radiochemical neutron activation analysis method for the determination of 22 elements in high-purity tungsten has been developed. For the assay of indicator radionuclides with long half-lives, the radiochemical separation was performed from HF/H₂O₂, HF/NH₄F and HCl/H₂SO₄ media by a combination of cation and anion exchange on a Dowex 50 W × 8 and Dowex 1 × 8 column. An effective removal of the matrix-produced radionuclides of W and Re was achieved. U was determined via ¹⁴⁰La, the daughter nuclide of the fission product ¹⁴⁰Ba. Limits of detection of 2 ng/g for U and 0.02 ng/g for Th can be achieved. For the other elements, the limits of detection are between 0.004 ng/g (Sc) and 200 ng/g (Sr). The elements Hf, Ta and Sb could be determined by instrumental neutron activation analysis. This method was applied to the analysis of two tungsten powder samples of different purity grade. The results and limits of detection are compared with those of other methods.     

An improved radiochemical neutron activation analysis procedure for trace mercury

Summary Radiochemical neutron activation analysis has proven to be a powerful tool for measuring trace mercury in a variety of materials. In a modification of an established NIST method, selenium interfering with the ²⁰³Hg indicator is removed by precipitating mercury as periodate, and the chemical yield is measured gravimetrically. The current method is better suited to multiple samples, less subject to explosion during the combustion step, provides a measurement of the yield for each sample, and involves less radiation exposure to personnel. The procedure has been applied to the certification of mercury in SRMs 1575a Pine Needles, 1632c Bituminous Coal, and 2702 Marine Sediment.     

Determination of rare earth elements in recent and fossil shells by radiochemical neutron activation analysis

Seven rare earth elements (La, Ce, Sm, Eu, Tb, Yb and Lu) in marine shell samples were determined by neutron activation analysis. In order to measure γ-ray using a Ge(Li) detector without serious interference from the intense Compton background from²⁴Na, a simple radiochemical separation was performed by a co-precipitation method with hydrated iron(III) oxide. The chemical yields for shell samples (91–99%) were determined by a re-activation technique for Gd and Yb. The interference from the²³⁵U(n, fission) reaction was corrected for determination of La and Ce. The data obtained in this study showed the behavior of rare earth elements in shells during the process of fossilization.     

Determination of trace siderophile elements in rock and meteorite samples by radiochemical neutron activation analysis

A simple and effective radiochemical procedure for radiochemical neutron activation analysis (RNAA) of ultra-trace siderophile elements (Ru, Re, Os and Ir) and rare earth elements (REEs) in rock and meteorite samples is presented. To design the procedure, several separation schemes of siderophile elements were examined by using radioactive tracers. By applying the procedure to rock and meteorite samples, we have determined Ru, Re, Os, Ir and REEs, and confirmed that our values were in agreement with the literature values. Our detection limits for Ru, Re, Os, La, Sm and Eu are significantly low compared with those for ICP-MS.     

Determination of impurities in tantalum by a radiochemical neutron activation analysis

A radiochemical separation method using Dowex 1×8 (200–400 mesh) has been applied to two tantalum metals of 99.9% purity. While tantalum was still retained on the resin, the elements Na, K, Cr, Mn, Fe, Co and Zn were separated with 2M HF and subsequently the elements Sc, As, Zr, Mo, Eu, W and Hf with a mixture of 0.5M HF and 3M HCl. The separation yields for all impurities was 98–100%. Elemental contents were calculated by a single comparator method using two monitors.     

Determination of ten trace elements in meteorites and lunar materials by radiochemical neutron activation analysis

A procedure is reported for the determination of Ni, Ge, Ru, Au, Ir, Zn, Ga, Cd, In and U in meteorites and lunar materials. The precision in multiple determinations at the 95% confidence level is less than 10% except for gold (15%). Ruthenium and uranium are determined by counting ⁹⁷Ru and ¹⁰³Ru x-rays; the chemical yield is determined from ¹⁰⁶Ru added before sample dissolution. The activity of ^116mIn is determined with improved sensitivity from integral counts in the region 1.5–3.0 MeV on a NaI(TI) detector.     

Multielement radiochemical neutron activation analysis of high purity aluminium

Summary A radiochemical neutron activation analysis technique for the determination of 51 elements in high purity aluminium via medium- and long-lived indicator radionuclides has been developed. It is based on a separation procedure involving the removal of ²⁴Na, produced via the reaction ²⁷Al(n,), on a hydrated antimony pentoxide column and further separation of the radionuclide mixture into 11 groups on two Dowex 1X8 columns and one Dowex 50X8 column from HCl/HF and HCl media as well as the extraction of copper with APDTC in chloroform. The indicator radionuclides for the significant impurities thorium and uranium, ²³³Pa and ²³⁹Np, were separated with satisfactory selectivity in one fraction. For 43 elements, the limits of detection are <10 ng/g, for thorium and uranium, they are 50 pg/g. The method was applied to the analysis of different high purity aluminium samples. For a number of elements, the results of this technique are compared with those of other techniques.

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Radiochemische Multielement-Neutronenaktivierungsanalyse von hochreinem Aluminium

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Dedicated to Prof. Dr. W. Fresenius on the occasion of his 75th birthday     

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 of some elements by epithermal neutron activation analysis for the Arctic aerosol

Summary We have determined nineteen trace elements in 685 aerosol filter samples collected during 1964-1978 in northern Finland by the Finnish Meteorological Institute. In this paper we present some procedures and results for very short (~25 s), short (~3-54 min), and medium (12-35 h) lived isotopes as determined by epithermal NAA in conjunction with and without Compton suppression. Elements with a I_γ/σthratio are favorable to be determined by epithermal NAA. Silver was determined by a one minute epithermal irradiation because of a very short ¹¹⁰Ag half-life. Antimony, arsenic, cobalt, bromine, indium, iodine, potassium, silicon, tin, tungsten, and zinc were determined by a ten minute epithermal irradiation. For silver determination, samples were counted without transferring the filter from the irradiated vial, however, for ten minute irradiation all samples were transferred to a non-irradiated vial and counted both in the normal and Compton mode by the HPGe gamma-spectrometry system with a decay time of about 10 minutes and counting time of 15 minutes. Each day a maximum of 16 samples were irradiated and immediately following the short counting, these samples were loaded into an automatic sample changer in sequence of irradiation and counted for an hour in both normal and Compton modes. This has proven to be an extremely cost effective measure thus reducing the need to employ long-lived NAA to analyze other elements such as Ag, Co, Sn and Zn and Ag for air pollution source receptor modeling.     

Multielement analysis by sequential instrumental and radiochemical neutron activation

We measured 37 elements in six USGS geological camples and one NBS biological orchard leaf (OL) sample, using sequential INAA and radiochemical group separation coupled with high resolution, high efficiency Ge(Li), and a Ge(Li) with anticoincidence shields. The elemental concentrations in these samples vary over three orders of magnitude. Our results agree very well with the reported values. The rare earth values in PCC-1 are 2–4 times lower than the reported values. Precise REE patterns are defined in USGS samples, which are characteristic of the total rock types. The REE pattern in OL is identical to the mineral apatite. In addition to the possibility that OL may be contaminated by local soil, it is also possible that the uptake of REE trace elements by plants from soil is perhaps dominated by accessory mineral such as apatite, or plants take up the REE from bulk soil in a preferential manner as a smooth function of the REE ionic radii.     

Precise trace rare earth analysis by radiochemical neutron activation

A rare earth group separation scheme followed by normal Ge(Li), low energy photon detector (LEPD), and Ge(Li)−NaI(Tl) coincidence-noncoincidence spectrometry significantly enhances the detection sensitivity of individual rare earth elements (REE) at or below the ppb level. Based on the selected γ-ray energies, normal Ge(Li) counting is favored for¹⁴⁰La,¹⁷⁰Tb and¹⁶⁹Yb; LEPD is favored for low γ-ray energies of¹⁴⁷Nd,¹⁵³Sm,¹⁶⁶Ho and¹⁶⁹Yb; and noncoincidence counting is favored for¹⁴¹Ce,¹⁴³Ce,¹⁴²Pr,¹⁵³Sm,¹⁷¹Er and¹⁷⁵Yb. The detection of radionuclides^152mEu,¹⁵⁹Gd and¹⁷⁷Lu is equally sensitive by normal Ge(Li) and noncoincidence counting;¹⁵²Eu is equally sensitive by LEPD and normal Ge(Li); and¹⁵³Gd and¹⁷⁰Tm is equally favored by all the counting modes. Overall, noncoincidence counting is favored for most of the REE. Precise measurements of the REE were made in geological and biological standards. Prepared for the U.S. Department of Energy under Contract DE-AC06-76RLO 1830.