Studies of kidney stones using INAA,EDXRF and XRD techniques

Four kidney stones collected from patients being treated in the Advance Urology Centre of PGIMR, Chandigarh were characterized using instrumental neutron activation analysis (INAA), energy dispersive X-ray fluorescence (EDXRF) and X-ray diffraction (XRD) techniques. For INAA, samples were irradiated in tray rod facility of Dhruva reactor, Mumbai and pneumatic fast transfer system of KAMINI reactor, IGCAR, Kalpakkam. Radioactive assay was carried out using HPGe detector coupled to 8k channel analyzer. Elements determined in the samples by INAA are Zn, Sr, Co, Fe, Cr, Sc, Se, Na and Mn. EDXRF was used for the quantification of Ca. XRD patterns showed that three of the kidney stones are calcium oxalate stone and the other one is uric acid stone. The concentrations of trace elements in general were found to be higher in calcium oxalate stones and positive correlation was observed in the concentrations of Ca with Sr and Zn.     

Role of diet and trace elements in lithogenesis of renal calculi

Twenty eight stones were characterized for chemical composition and structure. The concentrations of trace elements were determined using INAA while EDXRF was used for determining the calcium contents of the stones. Twenty stones were found to be mainly composed of calcium, six were mixed type and the remaining two were of uric acid type. The concentrations of trace elements namely Zn, Sr, Fe and Cr were lower in uric acid stones as compared to calcium based stones. Diet analysis of 310 patients who were treated for renal stones showed a diet rich in calcium and oxalate and decreased water consumption.

     

Chemical characterization of soda-lime glass samples by in situ current normalised PIGE and conventional INAA methods for forensic applications

Nuclear analytical methods namely in situ current normalised Particle Induced Gamma Ray Emission (PIGE) and conventional Instrumental Neutron Activation Analysis (INAA) were utilized for determining major, minor and trace concentrations of eighteen elements in five soda-lime (automobile) glass samples. Concentration of four major elements (Si, Na, Mg and Al) by PIGE and fourteen elements including ten trace elements by INAA were determined. For forensic application, major elements were used for confirming the class of glass samples, whereas concentration results of trace elements like transition and rare earth elements were utilized for finding similarity or differences among the glass samples.

     

Instrumental neutron activation analysis of carbonatites from Panda Hill and Oldoinyo-Lengai, Tanzania

Twenty nine (major and trace) elements including nine rare earth elements (REE) in African carbonatite samples were determined by instrumental neutron activation analysis (INAA). The geochemical behavior of trace elements in carbonatites, especially REE pattern (chondrite normalized), and the efficiency of neutron activation analysis compared to other methods are discussed in this study.     

Determination of protein-bound trace elements in bovine kidneys

Concentrations of up to 16 elements have been determined in subcellular fractions of bovine kidney using INAA methods. Levels of Rb and Se have been measured by a cyclic INAA method. A conventional INAA method consisting of 2 irradiations and 3 counting periods has been employed to determine the other elements. Accuracy of measurements has been evaluated by analyzing several standard reference materials. Trace element content of reagents used has been investigated in detail. Fresh samples of bovine kidney have been homogenized in a buffer containing sucrose and HEPES, and the homogeneate separated into nuclei, mitochondrial, lysosomal, microsomal and cytosol fractions by successive differential centrifugation. Concentrations of trace elements have been measured in these fractions using the INAA methods.     

Determination of trace element levels in polyethylene by instrumental neutron activation analysis

Elements Al, As, Au, Br, Cl, Co, Cr, Cu, Fe, Hg, K, La, Mn, Mo, Na, Sb, Sc, Sm, V, and Zn were determined by INAA in several brands and batches of high pressure polyethylene (PE) Bralen (Slovnaft Bratislava, Czechoslovakia). A large scatter of trace element contents was found in both granules and foils, indicating an inhomogeneous distribution for the majority of the above mentioned elements present as impurities in PE. Larger amounts of the elements Al, Mn, and Sb were found in foils than in granules. Blank values resulting from using of PE Bralen as a canning material for INAA were compared to trace element concentration in human hair samples, too.     

Spatial distribution of major and trace elements in bladder and kidney stones

The spatial distribution of major and trace elements has been studied in a range of human kidney and bladder stones with well documented histories to understand their initiation and formation. The stones were cut in half using a clean diamond saw and further cleaned, to remove surface contamination, in an ultrasonic bath. The cut surfaces were analyzed using laser ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS). The spatial distribution of Li, B, Mg, Al, P, Ca, Cr, Mn, Zn, Rb, Sr, Ba and Pb has been determined across the width of each stone.     

Determination of rare earths and other trace elements in samples of Antarctica by neutron activation analysis

The concentrations of REE and other trace elements have been determined in samples of Antarctica by Instrumental Neutron Activation Analysis (INAA). The samples were collected from the West Lake area near Great Wall Station. The samples include sediment, residual plants, rock and soil taken from the bottom of the lake to 3.4 m deep. The amounts of samples were very rare. In order to get more information, reactor NAA using both short and long irradiations with K₀ standardization has been adopted. Nine rare-earth elements (REE) namely La, Ce, Nd, Sm, Eu, Tb, Dy, Yb, and Lu as well as other trace elements (As, Au, Ba, Br, Co, Cr, Hf, Sc, Se, Th, V, Zn) have been determined. The concentrations and distribution patterns of REE in the samples have been given.     

Behaviour of trace element concentration in human organs in dependence of age and environment

To study the behaviour of trace elements in dependence of age and environment, samples of skin, lung, heart, aorta, kidney, liver, and brain were assayed for concentrations of Fe, Zn, Rb, Co, Cr, Se, Sc, Sb, Cs, Al and partly Eu. Nearly all element concentrations changed with progressing age, but they showed no clear correlation to either parameter assessed. The non-essential elements Sc, Sb, and Sc were increasingly concentrated in all organs except the skin. Comparing lung samples of patients from highly industrialized regions with those of lesser industrialization, the elements Sc, Al, Sb, Eu and Co were accumulated by a factor of 10 to 100. Thus the concentrations of trace elements in human organism also depends on the degree of industrialization.     

Multivariate analysis applied to some elements in human fluids and whole bloods of hemodialysis patients determined by INAA

This research is a framework of a big project aimed to the knowledge of human metabolism in hemodialysis patients. For reaching high sensitivity and obtaining accurate values for elements at very low concentrations Instrumental neutron activation analysis (INAA) was used for its characteristics to be a primary analytical method and because it does not require any chemical–physical pretreatment. The samples analyzed (160) are representative of groups of homogeneous population and specific matrices (hemodialysis fluids and whole human blood). The irradiation was performed in the rotating rack (Lazy Susan) of the Triga Mark II reactor of the R.C. Casaccia-ENEA at a neutron flux of 2.6 × 10¹² n cm^?2 s^?1 with an irradiation time of 12 h. The results on the hemodialysis fluids report the values and the behavior of selected trace elements: the levels of Br and Na show a decrease between the pre- and post-dialysis whereas Fe, K and Zn an increase. The other elements such as Cs, Rb and Se seem to keep constant between the two phases. Similar data are found for the whole human blood for the same selected elements. Finally, exploiting the INAA peculiarity it has been investigated the levels of trace and ultra-trace elements interesting from a toxicological (Hg, Ni, Sb) and nutritional (Co, Cr) point of view and seldom determined due to their analytical implications. Finally, a chemiometric investigation performed through dendrogram trees, Canonical discriminant analysis and principal component analysis, has evidenced the similar effects of the HF, HDF and BIC-treatments on the investigated fluids respect to the CAPD dialysis.     

Rare earth element patterns in ultramafic rocks of the Schist Belt of Southwestern Nigeria by instrumental neutron activation analysis

24 Ultramafic rock samples from 3 different areas of the Schist Belt of Southwestern Nigeria were analyzed for 11 rare earth elements (REE) by instrumental neutron activation analysis (INAA). REE patterns of the ultramafic rocks are similar for the 3 different areas, and the REE abundances are smaller than for other types of rocks from the same areas. However, the moderate fractionation between LREE and HREE observed for these samples is unusual for ultramafic rocks. Some geochemical implications of the results are discussed.     

The non-destructive determination of REE in fossilized bone using synchrotron radiation induced K-line X-ray microfluorescence analysis

The sensitivity and applicability of the synchrotron radiation induced X-ray microfluorescence (μ-SRXRF) spectrometer at the Hamburg synchrotron laboratory Hasylab for the determination of the distribution of trace concentrations of rare-earth elements (REE) in fossilized bone are discussed and critically compared to those of other trace analytical methods such as instrumental neutron activation analysis (INAA) and LAMP-ICPMS (laser ablation microprobe inductively-coupled plasma mass spectrometry). Measurements were carried out on two bone samples from contrasting terrestrial depositional environments at Olduvai Gorge (Tanzania). Results indicate that the microdistribution of the REE in these biological materials is not homogeneous and that the relative abundance of these elements can provide information on the palaeoenvironment during the fossilization process. The heterogeneous distribution of the REE can be determined in a quantitative and completely non-destructive manner provided the concentrations of individual REE are above 10 μg/g.     

Trace element concentration differences in regions of human brain by INAA

Studies have shown that there is a potential relationship between the levels of trace elements in cerebral tissues and neurological disorders. However, there are few publications available on the elemental composition of these tissues as well as for different regions of the brain. The aim of this study was to investigate trace element differences in various regions of the human brain from an elderly population of normal individuals. Brain samples from 31 individuals of both genders, aged 51–95 years were provided by the Brain Bank of the Brazilian Aging Study Group of the São Paulo University, Medical School. The tissues from the regions of the hippocampus, cerebellum and frontal, parietal, temporal, occipital cortex were dissected using a titanium knife, ground, freeze-dried and then analyzed by instrumental neutron activation analysis (INAA). Samples and element standards were irradiated with a neutron flux at the IEA-R1 nuclear research reactor for Br, Fe, K, Na, Rb, Se and Zn determinations. One-way ANOVA test (p < 0.05) was used to compare the results which showed significant differences for several elements among the brain regions. Most of our brain analysis results agreed with the literature data. The results were also submitted for brain region classification by cluster analysis.     

Instrumental neutron activation analysis of some rock samples from Akwana and Arufu areas,Middle Benue Trough,Nigeria

Twenty nine (29) major, minor and trace elements including rare earth elements (REEs) were determined by INAA in rock samples from Akwana and Arufu areas, Middle Benue Trough, Nigeria. The rock units are located within the lead-fluorite and baryte mineralisation there. The concentrations of the major elements in the tertiary basalt (TB) and dolerite are similar while the elemental abundance in the granite gnesses is completely different. The elemental concentrations in the rock samples do not show any known relationship with fluorite abundance. The concentrations of some elements in both tertiary basalt and dolerite show them to be derived from alkali basaltic liquid. The chondritic normalised REE distribution patterns for the TB are similar to those of BCR-1 but the chondritic relative REE abundance is more enriched in TB than in the BCR-1. The chondritic normalised REE distribution patterns for the granite gneisses are also compared to those of the standard granite samples.     

The use of neutron activation in dietary reference material analysis

Summary Results for a number of trace elements in a total human diet material (USDIET-1), obtained by the application of both INAA and RNAA are presented. Several dietary reference materials such as NBS SRM 1577A, and BCR CRM Single Cell Protein were also analyzed, and these results are also given. Combining measurements on short and long lived radionuclides, the INAA approach is useful for the determination of about 20 elements. In order to expand the elemental coverage or improve detection limits, RNAA was also explored in two modes: separation of radionuclides using organic ion exchange resins and the use of hydrated manganese dioxide. This combination is applicable to 15 trace elements. For example, using RNAA, the following results were obtained for USDIET-1: Cd=31.8, Mo=280, Cr=71, Ag=4, As=117 and Sb=9.4 g/kg. In the INAA mode, special attention was given to Al, F and Se. The F content of USDIET-1 was found to be 840 mg/kg, a rather high value, resulting from handling USDIET-1 by Teflon tools. By applying INAA and RNAA under two different laboratory conditions, it has been demonstrated that, even for the so-called difficult to determine elements like Cr, As or Mo, consistent results can be obtained. Thus, NAA promises to be a strong tool for human nutritional studies.

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Einsatz der Neutronenaktivierung für Nahrungsmittel-Referenzmaterialien

     

Trace elements in head hair of hemodialysis patients

Instrumental neutron activation analysis /INAA/ was applied to measure trace elements in head hair of 19 patients with impaired renal function /14 males and 5 females/ and of 40 normal individuals /20 males and 20 females/. It was the aim to use head hair as a possible indicator of total body trace elements status and to investigate whether significant changes occur as a result of chronic hemodialysis. The elemental concentrations of 20 elements /i.e. Na, Mg, Al, Cl, K, Ca, V, Mn, Fe, Co, Cu, Zn, As, Se, Br, Ag, Cd, Sb, I and Au/ are presented and compared with published data. The present study revealed that the hair of the dialysis patients contained about ten times more iodine than that of the control group. No significant differences were observed for the other elements measured, except for sodium and antimony.     

Elemental analysis of the frontal lobe of “normal” brain tissue and that affected by Alzheimer's disease

Normal brain tissue and brain tissue affected by Alzheimer's disease has been taken from the frontal lobe of both hemispheres and their elemental compositions in terms of major, minor and trace elements compared. Brain samples were obtained from the MRC Alzheimer's Disease Brain Bank, London. 25 samples were taken from 18 individuals (5 males and 13 females) of mean age 79.9±7.3 years with pathologically confirmed Alzheimer'sdisease and 26 samples from 15 individuals (8 males and 7 females) of mean age 71.8±13.0 years with no pathological signs of Alzheimer's disease (normals). The elemental concentration of the samples were determined by the techniques of Rutherford backscattering (RBS) analysis, particle induced X-ray emission (PIXE) analysis and instrumental neutron activation analysis (INAA). Na, Mg, Al, Cl, K, Sc, Fe, Zn, Se, Br, Rb and Cs were detected by INAA and significant differences in concentrations were found between concentrations in normal and Alzheimer tissue for the elements. Na, Cl, K, Se, Br and Rb, P, S, Cl, K, Ca, Fe, Zn and Cd were detected by PIXE analysis and significant differences found for the elements P, S, Cl, K and Ca.     

Thermal, UV, FTIR, and XRD studies of urinary stones

Various crystals are seen in human urine. Oxalate, Phosphate, Uric acid, and Urate crystals are generally seen in urinary calculi. Calcium stones are most common, comprising 75 % of all urinary calculi. They may be pure calcium oxalate or calcium phosphate or a mixture of both. Many stones are not homogeneous. Low calcium intake increases the intestinal absorption of calcium, thus decreasing the amount of calcium available in the intestinal tract to form insoluble complexes with Oxalate. Consequently, a higher amount of oxalate is available for intestinal absorption and as a result, urinary oxalate excretion increases. Mineral water consumption did not reduce urinary oxalate excretion. High urinary excretion and concentration of magnesium decrease both the nucleation and growth rates of calcium oxalate crystals in urine, because of the higher solubility of magnesium oxalate compared with calcium oxalate. Analytical results show calcium oxalate to be one of the major inorganic components of renal stones and found to be present in almost all kidney and bladder stones. About 39.5 % of the total composition of the calculi is found to contain purely calcium oxalate and also hydroxyl apatite. The ten samples are a mixture of calcium oxalate and phosphate stones. Four samples are calcium oxalate as major composition and the remaining are calcium phosphate as major composition. These kidney stones are taken photographically and size of the stone are measured using optical microscopy. These qualitative analyses are also confirmed by UV, FTIR, DSC, and XRD analysis.     

Concentrations of rare earth elements in sediments,mussels and fish from a Danish marine environment,Lillebaelt

Results for the content of the rare earth elements (REE), La, Ce, Nd, Sm, Eu, Tb, Yb and Lu in sediments, mussels and fish are presented for an area polluted by REE. The REE are emitted with the process waste water stream from a fertilizer production plant. The method of analysis has been INAA. An attempt to combine the INAA with a simple destruction/preconcentration method is described.     

The non-destructive determination of REE in fossilized bone using synchrotron radiation induced K-line X-ray microfluorescence analysis

The sensitivity and applicability of the synchrotron radiation induced X-ray microfluorescence (μ-SRXRF) spectrometer at the Hamburg synchrotron laboratory Hasylab for the determination of the distribution of trace concentrations of rare-earth elements (REE) in fossilized bone are discussed and critically compared to those of other trace analytical methods such as instrumental neutron activation analysis (INAA) and LAMP-ICPMS (laser ablation microprobe inductively-coupled plasma mass spectrometry). Measurements were carried out on two bone samples from contrasting terrestrial depositional environments at Olduvai Gorge (Tanzania). Results indicate that the microdistribution of the REE in these biological materials is not homogeneous and that the relative abundance of these elements can provide information on the palaeoenvironment during the fossilization process. The heterogeneous distribution of the REE can be determined in a quantitative and completely non-destructive manner provided the concentrations of individual REE are above 10 μg/g. Received: 18 January 1998 / Revised: 6 October 1998 / Accepted: 10 October 1998