Simultaneous PIXE/PIGE was used to determine the concentration of 20 elements including N, O, F, Na, Mg, P, Ca (PIGE) and Cr, Mn, Cu, Zn, Cd, Ba, Pb (PIXE) in a number of animal and human rib samples, marrow, and the IAEA CRM Animal Bone (H-5). Samples and standards were bombarded with 2.5 and 4.0 MeV external proton beams. The minimum detection limits for most of the minor and trace elements ranged from 0.5 to 1.5 ppm. The sample preparation procedure for the nondestructive instrumental analysis of bone is discussed in detail. The analysis method is fast, nondestructive and offers selective analysis of the cortical and cancellous surface of the same bone sample.
A radiochemical solvent extraction method has been developed for the simultaneous determination of submicrogram amounts of Cd and Hg using115mCd and203Hg tracers respectively and thionalide as a single complexing reagent. Hg was determined by 0.05% thionalide in ethyl methyl ketone (EMK) at pH 8.5, masking Cd with 0.1M KCN. From the aqueous phase Cd was demasked using formal-dehyde-acetic acid, pH adjusted to 9.5 and extracted into 0.05% thionalide in chloroform. The method is simple, fast and yields accurate results.
Instrumental Neutron Activation Analysis /INAA/ has been employed for the determination of 15 major, minor and trace elements in human and animal blood samples. Dry whole blood samples along with NBS and IAEA standards were irradiated for 5 min, 1 h, 5 h and 10 h with reactor thermal neutrons and counted using high resolution -spectrometry at successive intervals. Data for a new IAEA proposed CRM Mixed Human Diet /H-9/ is reported.
Instrumental Neutron Activation Analysis (INAA) has been employed for the multielemental determination of an IAEA intercomparison standard Hay Powder, V-10 and some edible plant leaves consumed in India. The samples were irradiated with thermal neutrons at a flux 1012 n·cm–2·s–1 in a reactor for 5 minutes, 1, 2, 5, 10 and 15 hours and counted by high resolution -ray spectrometry. Nearly 18 elements have been determined. Good agreement is observed for most of the elements in several NBS standards and the proposed CRM V-10. Some edible vegetable plant leaves have also been analyzed.
A radiochemical solvent extraction method has been developed for the micro determination of Mo/VI/ using99Mo tracer. It involves removal of99mTc by ethyl methyl ketone /EMK/ and extraction of Mo with tri-n-butyl phosphate /TBP/ from 5M HCl. Different parameters affecting the extraction such as pH dependence, nature of solvent and interferences due to other radionuclides have been studied. The method can be used up to 2 g of Mo.
Phosphorus has been determined using the
- emitter32P by instrumental neutron activation analysis (INAA) in several NBS and IAEA standards and samples of biological origin such as human and animal blood, cancerous tissue, edible plant leaves, diets, milk samples, etc. The method involves thermal neutron irradiation for 2–10 h in a reactor followed by
--counting on an end-window gas flow proportional counter using an aluminium filter. The results are within ±10% of the certified values in most cases.
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.
Short-term reactor irradiation followed by successive counting over long periods has been used for the nondestructive determination of more the 20 elements in geological and biological samples. The samples, along with USGS standards and NBS SRMs, were irradiated for 5 m, 10 m, 15 m, 1 h, 2.5 h, and 10 h, followed by counting on a Ge/Li/ gamma-ray spectrometer. The technique has been employed for the determination of several major, minor, and trace constituents in geological, biological and environmental samples.
A radiochemical solvent extraction method has been developed for the determination of Mn(II) using54Mn tracer. Mn(II) is complexed with 2-thenoyltrifluoroacetone (TTA) at pH 8.5 and extracted in isobutyl methyl ketone (IBMK). Different parameters affecting the extraction, and interferences due to diverse ions have been studied. The method can be used for the determination of Mn in microgram amounts.
Authors:C. Cornett, D. Samudralwar, W. Ehmann, and W. Markesbery
The possible association of dental amalgam surface exposure, brain mercury (Hg) levels, and pathological markers of Alzheimer's disease (AD) in the brain is the subject of an on-going study in our laboratory. Two radiochemical neutron activation analysis methods and the use of instrumental neutron activation analysis (INAA) with Compton suppression spectrometry have been evaluated for improving our INAA Hg detection limit (2.8±0.6 ng/g, wet-weight basis) in human tissue. Large numbers of samples dictated the use of a purely instrumental method or rapid, simple radiochemical separations. Human brain tissues and NIST biological standards were analyzed using a precipitation of Hg2Cl2, a solvent extraction utilizing sodium diethyldithiocarbomate, conventional INAA, and INAA with Compton suppression. The radiochemical precipitation of Hg2Cl2 proved to be the most useful method for use in our study because it provided a simultaneous, quantitative determination of silver (Ag) and a Hg detection limit in brain tissue of 1.6±0.1 ng/g (wet-weight basis).