Accumulation and distribution of elements in rice /seed,brand layer,husk/ by neutron activation analysis

Various rice samples /seed, brand layer, husk/ from Vietnam were analyzed for Se, Hg, Cr, Ni, Sc, Rb, Fe, Zn and Co by neutron activation analysis. The concentration values found /seed/ were the following: Se 0.04–0.07 ppm, Hg 0.02–0.07 ppm, Cr 2.13–8.65 ppm, Ni 1.56–4.95 ppm, Sc 0.02–0.06 ppm, Rb 0.84–2.71 ppm, Fe 26.31–96.07 ppm, Zn 10.65–27.39 ppm and Co 0.02–0.15 ppm. The values were reported in ppm /dry weight/. Statistical analysis /t-test, t=0.05/ showed that the content of elements varies between sorts of rice; the content of Rb, Fe, Ni, Cr of rice husk was significantly higher than in rice seed and brand layer.     

Trace elements analysis in rice

Various rice species, marketed in Austria, were analyzed for their Se, Cr, Ni, Rb, Fe, Co, Cs, Ag and Hg contents by neutron activation analysis. The concentration values found for Se ranged between 0.023 and 0.265 ppm, for Cr 0.540–1.875 ppm, for Ni 0.359–0.965 ppm, for Rb 1.604–6.400 ppm, for Fe 24.3–139.8 ppm, for Co 0.026–0.055 ppm, for Cs 0.016–0.032 ppm, for Ag 0.0006–0.0034 ppm, for Hg 0.003–0.023 ppm. Statistical analysis showed in the majority of cases that there is a significant difference in Se, Cr, Ni, Rb, Fe, Co, Hg contents but not in Cs. Highest values of Se and Fe were found in rice from Belgium /long seed, super patna/, whereas the Cr concentration was the highest in rice from Thailand /siam patna/. Ni was highest in rice from Uncle Ben's, Rb in Kresto from USA.     

Estimation of trace metals in pure graphite by emission spectroscopy

Summary A direct emission spectrographic method for the estimation of Al, B, Ca, Cd, Co, Cr, Fe, Mg, Mn, Mo, Ni, Pb, Si, Sn, V and Zn in graphite at ppm concentrations has been developed. The effect of different carriers, was investigated and NaF at 1% concentration was found most suitable for the estimations. Ten milligram charge of standards and samples contained NaF as carrier and palladium as internal standard. The spectra were excited in d.c. arc carrying 13 amp current for 25s and photographed on 3.4 M Ebert Grating Spectrograph, on S.A.1 plates in the region 2200–3400 Å. The detection limits lie in the range of 0.25–10 ppm for different elements analysed with precision of 20% or better. The limits obtained here for Ca, Co, Fe and Zn are lower than those reported earlier in the literature.

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Emissionsspektrographische Bestimmung von Metallspuren in reinem Graphit

Zusammenfassung Eine Methode zur direkten Bestimmung von Al, B, Ca, Cd, Co, Cr, Fe, Mg, Mn, Mo, Ni, Pb, Si, Sn, V und Zn im ppm-Bereich in Graphit wurde ausgearbeitet. Verschiedene Trägermaterialien wurden geprüft und 1% NaF wurde als optimal gefunden. Palladium diente als innerer Standard. Zur Anregung wurde der Gleichstrombogen benutzt (13A, 25s; 3,4M Ebert Gitta-Spektrograph, S.A. 1 Platten, 2200–3400 Å). Die Nachweisgrenzen liegen im Bereich von 0.25–10 ppm (Genauigkeit 20% oder besser). Die Nachweisgrenzen für Ca, Co, Fe und Zn sind niedriger als die bisher in der Literatur beschriebenen.

     

Determination of arsenic,scandium, chromium,cobalt and nickel in asbestos by neutron activation analysis

Arsenic, scandium, chromium, cobalt and nickel were determined by neutron activation analysis in various Chrysolite-Asbestos from Canada, Russia, Italy in an asbestos plate, and in dry, as well as in wet manufactured asbestos. Following concentration values were found: for As 0.01–5.5 ppm, for Sc 5.4–14.80 ppm, for Cr 79.5–918.8 ppm, for Co 10.8–80.9 ppm, for Ni 148–1786 ppm. Statistically significant differences /t=0.05/ in contents of As, Sc, Cr, Co and Ni were detected in the different samples of asbestos. The concentration of As and Cr in Italian asbestos were considerably higher than in Canadian chrysolite.     

Daily dietary intake of trace elements of radiological and nutritional importance by the adult Indian population

The concentrations of eleven trace elements: Ca, Co, Cr, Cs, Fe, I,K, Se, Sr, Th and Zn were determined in total diet samples and also in individualfood materials which constitute the typical Indian diet. Instrumental neutronactivation analysis (INAA) and radiochemical neutron activation analysis (RNAA)were employed for the analysis. Whereas the elements Fe, Co, Cr, Se and Znare important from the view point of their role in nutrition, the elementsCs, K, Sr and Th are of importance in radiation protection, and Ca and I havedual importance: both in nutrition as well as in radiation protection. Basedon the analysis of twenty total diet samples, prepared as per the data onthe dietary intake pattern of four provinces of India and the data on intakepattern of an average adult Indian, the geometric mean (GM) intake of variouselements was estimated to be 0.33 g (0.2–0.67) for Ca, 16.5 µg(8.3–31.1) for Co, 52.3 µg (35.1–131) for Cr, 4.7 µg(2.79–11.8) for Cs, 94.6 µg (60.6–201) for I, 1.90 g (1.25–3.54)for K, 1.13 mg (0.78–2.97) for Sr, 0.76 µg (0.45–1.66) forTh, 15.9 mg (10.2–34.3) for Fe, 56.3 µg (27.6–105.3) forSe and 8.6 mg (5.1–16.7) for Zn. Some of the important individual foodmaterials, such as cereals, pulses, milk, vegetables etc., were also analysedfor these elements to observe the contributions of the individual food materialsto their daily dietary intake. The results of the analysis showed that inthe case of Cs, K, Sr, Th, Fe, Zn and Co, almost 50% of the daily dietaryintake of the above stated elements is contributed by cereals and pulses.In the case of Ca however, significant amount is contributed by milk and incase of I, iodised salt could make significant contribution. The data collectedso far, for Se and Cr, was not sufficient to draw any definite conclusion.     

AAS-Bestimmung von Eisen, Nickel, Kobalt, Mangan und Chrom in Wolfram und Molybd?n

Zusammenfassung Das Atomabsorptionsverhalten von verschiedenen Metallen (Fe, Ni, Co, Mn, Cr) in Wolfram und in Molybdän wurde untersucht. Eine gegenseitige Störung dieser Elemente wurde nicht beobachtet. Ferner wurde der Einfluß von Dopsubstanzen, wie Alkali, Calcium, Aluminium oder Silicium auf das Absorptionsverhalten untersucht. Die Metalle Fe, Ni, Co, Mn und Cr lassen sich ohne vorherige Trennungsoperationen in Wolfram oder Molybdän bestimmen. Die Empfindlichkeit betrug etwa 0,10–0,30 g/ml oder 5–20 ppm im festen Metall.

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AAS-determination of iron, nickel, cobalt, manganese and chromium in tungsten and molybdenum

Results of the atomic-absorption behaviour of several metals (Fe, Ni, Co, Mn, Cr) in tungsten and in molybdenum are reported. No mutual interference of these elements has been observed. Furthermore the influence of dope-elements, as alkali, calcium, aluminium or silicon, has been investigated. AAS can be applied without prior separation procedure for the determination of Fe, Co, Ni, Mn and Cr in tungsten and in molybdenum. The sensitivity found was in the range 0.10–0.30 g/ml or 5–20 ppm in the solid material, respectively.

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Anerkennung. Für die sorgfältige Durchführung der Analysen danke ich Frau E. U. Stamer.     

AAS determination of Co, Ni, Mn and Cr in ores, concentrates and dusts from copper metallurgy after matrix elements separation by extraction

Summary A method has been developed for the AAS determination of Co, Ni, Mn and Cr in ores, concentrates and dusts of copper metallurgy at the 10^–3–10^–1% level. The matrix elements (Cu, Pb, Zn, Fe) were separated in a two-stage extraction: with MIBK from 6 M HCl solution and with 0.1 M tetrahexylammonium iodide (THAI) in MIBK from 3 M HCl, in form of ion-pairs, without Co, Ni, Mn and Cr losses. Values of r.s.d. were 2.0–6.0%.

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AAS-Bestimmung von Co, Ni, Mn und Cr in Erzen, Konzentraten und Stäuben aus dem Bereich der Kupfermetallurgie nach Abtrennung der Matrixelemente durch Extraction

Zusammenfassung Das beschriebene Verfahren eignet sich für den Bereich von 10^–3 bis 10^–1%. Die Matrixelemente (Cu, Pb, Zn, Fe) wurden als Ionenpaare ohne Verluste an Co, Ni, Mn und Cr mit Hilfe einer zweistufigen Extraktion abgetrennt: mit MIBK aus 6 M HCl-Lösung und mit 0,1 M Tetrahexylammoniumiodid (THAI) in MIBK aus 3 M HCl-Lösung. Die relativen Stadardabweichungen lagen im Bereich von 2,0 bis 6,0%.

     

Preconcentration and XRF-determination of heavy metals in hair from Sudanese populations

Energy-dispersive X-ray fluorescence analysis was applied for the analysis of hair. The hair samples were digested in a mixture of nitric and perchloric acid and the heavy metals were precipitated with ammonium pyrrolidine dithiocarbamate. The accuracy, precision and recovery of the method for the elements Fe, Ni, Cu, Zn and Pb were evaluated through the analysis of a standard hair sample. The procedure was applied to the analysis of hair from an occupationally exposed group of Sudanese workers and a control group. The hair of the exposed group showed a range of 80–550 ppm Fe, 6–12 ppm Cu, 57–190 ppm Zn and 70–3700 ppm Pb, while that of the control group had a range of 60–310 ppm Fe, 7–22 ppm Cu, 89–170 ppm Zn and 3–17 ppm Pb.     

Spectrographic estimation of impurities in selenium

Summary An emission spectrographic method for the estimation of impurities of Al, As, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Sn, Te, Ti, V, Zn and Zr in high purity selenium at concentrations less than 1 ppm has been developed. The impurities were separated from 1 g of selenium by volatilizing Se from its solution in nitric acid and sulphuric acid. The residue containing impurities was dissolved in small amounts of 6 M HCl and loaded along with the washing on 10 mg mixture containing graphite (90%) and sodium chloride carrier (10%), in the electrode crater. The spectra were excited in a d.c. arc carrying 13 A. The detection limits lie in the range 0.005–0.5 ppm for the different elements. The precision of the method ranges from 7–18% for these elements.

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Spektrographische Bestimmung von Verunreinigungen in Selen

Zusammenfassung Folgende Verunreinigungen werden in hochreinem Selen in Konzentrationen von <1 ppm bestimmt: Al, As, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Sn, Te, Ti, V, Zn und Zr. Das Selen wird von den Verunreinigungen durch Verdampfen abgetrennt (Lösen einer 1 g-Probe in HNO₃/H₂SO₄). Der Rückstand wird in 6 M HCl gelöst und zusammen mit einem Graphit/NaCl-Gemisch (9010) in die Elektrodenbohrung gefüllt. Die Anregung erfolgt in einem Gleichstrombogen von 13 A. Die Nachweisgrenzen liegen im Bereich von 0,005–0,5 ppm, die Genauigkeit beträgt 7–18%.

     

Neutron Activation Analysis of Bottom and Fly Oil Ash Leachates

Seven samples of oil fly and bottom ashes were leached with water using a Canadian standard test method for shake extraction of solid waste. The concentrations of 20 elements in the leachates were determined by the computerized systematic instrumental absolute neutron activation analysis. The ranges of concentrations (in ppm) found for the elements in the leachates were: Al (3–526), Ba (0.5–6), Ca (100–695), Cl (13–59), Co (1–6.3), Cr (0.2–6.6), Cs (0.03–0.4), Eu (0.003–0.01), Fe (28–690), K (42–464), La (0.3–49), Mg (214–3150), Mn (1.2–20), Na (88–4050), Sb (0.04–0.4), Sc (0.003–0.07), Sr (1.2–23), U (0.07–1), V (1.2–4540) and Zn (2.3–200). These findings were compared with the maximum concentrations allowed for these elements by Canadian regulations. The concentrations of Cr and U were found to be higher than their permissible limits on 7 occasions. The purpose of this study was to determine the background levels of different elements in oil ash leachates, in order to evaluate their potential impact on underground water.     

Determination of trace elements in honey by INAA in Turkey

Instrumental neutron activation analysis was applied to the determination of As, Cr, Sb, K, Br, Zn, Fe, Co in Turkish honey. Irradiation time was 6 h underwater at a thermal flux of 10¹³ n cm^–2 s^–1; cooling times of 100 h and 3–4 weeks and counting times of 5000 s and 80.000 sec were used. The detection limit for As is 0.01 ppm for honey matrix under these conditions. A technique was developed for sealing the quartz tube containing the honey with flame.     

Aktivierungsanalytische Bestimmung von Verunreinigungen in hochreinem Aluminium

Zusammenfassung Zur Bestimmung geringer Gehalte der Elemente Au, Hg, Cu, Cd, As, Sb, Sn, Ga, Fe, In, Cr, Co, Ni, Mn, Zn, Mo und W in hochreinem Aluminium wurde eine aktivierungsanalytische Methode ausgearbeitet. Bei einer Einwaage von insgesamt etwa 1 g kann die Analyse mit Nachweisempfindlichkeiten zwischen 1 · 10^–6 (Au) und 0,5 ppm (Fe) durchgeführt werden. Die erforderlichen chemischen Trennoperationen werden beschrieben.

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Summary A method is described for the determination of low contents of the elements Au, Hg, Cu, Cd, As, Sb, Sn, Ga, Fe In, Cr, Co, Ni, Mn, Zn, Mo and W in high-purity aluminium by activation analysis. With sample weights of about 1 g sensitivities are obtained between 1 · 10^–6 (Au) and 0,5 ppm (Fe). The chemical separation procedures required are described.

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Den Herren W. Schweighofer und U. Grahmann möchten wir an dieser Stelle für ihre wertvolle Mitarbeit hei der Ausarbeitung und Durchführung der Analysen danken.

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Herrn Prof. Dr. W. Geilmann zum 75. Geburtstag gewidmet.     

Determination of some trace elements (Fe,Co, Cr,Zn, Cu,Mn, and In) in different series of standard reference samples by neutron-activation analysis

Summary In this paper methods of determining traces of Fe, Co, Cr, Zn, Cu, Mn and In in standard reference materials by neutron-activation analysis are described. The maximum selectivity and sensitivity for measurements of these elements was obtained by combining ion-exchange, extraction and precipitation methods with use of an NaI(Tl) detector. After a long irradiation, addition of carriers and dissolution of samples, Fe, Co, Zn and Cr were separated on a Dowex 1X8 anion-exchange column from 10M HCl medium. Chromium passes through the column under these conditions and is separated from interferences by extraction of Cr₂O₇ ^2– with methyl isobutyl ketone. The other three elements are selectively eluted with HCl of different concentrations (5M, 0.5M, 0.01M). Cobalt and zinc are extracted as the dithiocarbamates from the fractions obtained, and iron with tributyl phosphate. Separation and determination of Cu, Zn, Mn and In as their short-lived isotopes is based on extraction of their dithiocarbamates into CCl₄ under specific conditions. The purity of the-spectra obtained, the high chemical yields and good reproducibility, indicate that these methods are suitable for determination of these trace elements in a wide spectrum of inorganic materials.

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Zusammenfassung Die Bestimmung von Spuren der Elemente Fe, Co, Cr, Zn, Cu, Mn und In in Standardvergleichsmaterialen mittels Neutronenaktivierungsanalyse wurde beschrieben. Mit einer Kombination von Ionenaustausch-, Extraktions- und Fällungsmethoden wurde eine maximale Selektivität und Empfindlichkeit mit dem NaJ/Tl Detektor erzielt. Nach einer längeren Bestrahlung, nach Zugabe von Trägersubstanzen und nach Auflösung der Proben wurden Fe, Co, Zn und Cr mit dem Anionenaustauscher Dowex 1X8 aus 10-n Salzsäure getrennt. Unter diesen Bedingungen wird Cr nicht adsorbiert. Von störenden Elementen im Eluat wird Cr in der Endphase durch Extraktion des Cr₂O₇ ^2– mit Hexon getrennt. Die übrigen drei Elemente eluiert man selektiv mit HCl verschiedener Konzentration (5-n, 0,5-n und 0,01-n). Aus den Fraktionen werden Co und Zn als Carbamate und Fe mit Tributylphosphat extrahiert.Trennung und Bestimmung von kurzlebigem Cu, Zn, Mn und In beruhen auf der Extraktion ihrer Carbamate mit CCl₄ unter spezifischen Bedingungen.Die Reinheit der erhaltenen Spektren, die hohen chemischen Ausbeuten und die gute Genauigkeit der Resultate beweisen, daß sich die beschriebenen Methoden zur Analyse zahlreicher anorganischer Materialien eignen.

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The paper was presented at the IV. Polish Conference on Analytical Chemistry, Warsaw, August 1974.     

Neutron activation analysis of major and trace elements in crude petroleum

We have determined the concentration of 25 trace elements in crude petroleum from seven Libyan oil fields by instrumental neutron activation analysis. Crude oil samples were irradiated with a thermal neutron dose rate of 10¹² and 10¹³ n·cm^–2·s^–1 in the Tajoura research reactor. The concentration of U, Br, Mg, Cu, Na, V, Cl, Al, Mn and Ca is in a range of 0.015 to 84 ppm and that of sulphur of 0.12 to 1.8%. The elements Sc, Cr, Ni, Fe, Co, Zn, Ag, Se, Sb, Ba, Cs, Yb, Hf and Hg have a concentration range of 0.009 to 8747 ppb. The coefficients of variation are within 10%. The elements V and Ni occur as both porphyrin and non-porphyrin and the ratio of these two forms varies over a wide range. The V/Ni ratios are located between 0.17 and 6.67, which are comparable to the reported values for the crude oils from other countries.     

Neutron activation analysis of asbestos from Canada

Concentrations of Al, Au, Br, Ce, Cl, Co, Cr, Fe, K, La, Mg, Mn, Na, Ni, Sb, Sc, Sm, Srm and V were determined in 6 samples of asbestos from Canada. They were equal to (in ppm): Al 1660–3430; Au 0.03–0.04; Br 3.1–11.7; Ce 1.7–4.8; Cl 116–331; Co 35–83; Cr 200–2060; Fe 29300–42200; K 125–867; La 0.28–1.03; Mg 24–25.9%; Mn 418–545; Na 364–1610; Sb 0.65–1.46; Sc 3.73–5.57; Sm 0.09–0.3; Sr 26.7–41.4; V 8.4–14.3. Five toxic elements were found in asbestos; Cr, Mn, Ni, Sb and V.     

Assessment of the essential element and heavy metal content of edible fish muscle

The aim of this work was to determine the concentrations of some essential and toxic elements in the muscle of ten species of commercial fish consumed in Portugal. We combined two different techniques for determination of the elements—energy-dispersive X-ray fluorescence (EDXRF) was used to quantify K, Ca, Fe, Zn, Se, Rb, and Sr and flame atomic-absorption spectrometry for analysis of Cr, Ni, Cu, Cd, Hg, and Pb. The latter technique was used because of its higher sensitivity, because these elements were not detected by EDXRF. The results obtained show a similar pattern for the trace elements. K and Ca are present at the highest concentrations in all the samples studied, from 0.6–1.3% and from 0.04–0.08%, respectively, followed by Zn, Fe, Sr, Se, and Rb. Sr is present at higher concentrations than Rb in all the species studied except meagre. Concentrations of the elements in octopus do not follow this pattern—Fe is present at a higher concentration than Zn. Low concentrations of Cr (0.66–1.5 g g^–1), Ni (0.11–0.24 g g^–1), Cd (0.01–0.08 g g^–1), Hg (0.49–2.74 g g^–1), and Pb (0.02–0.06 g g^–1) were observed in all the samples analysed. The concentration of Hg was highest in Helicolenus dactylopterus—5.4 g g^–1 in one sample.     

Trace element concentration in human gallstones using instrumental neutron activation analysis

The concentrations of trace elements in two types of gallstones in 24 female patients in Tripoli aged 24–60 years have been determined using instrumental neutron activation analysis. These elements are Co, Fe, Mn, Se and Zn. The results are expressed in ppm and are in agreement with reported values. The data suggested that the concentrations of trace elements increase with age.Presented at the MTAA-8 Conference, September 16–20, 1991, Vienna, Austria.     

Co-precipitative pre-concentration with sodium diethyldithiocarbamate and ICP-AES determination of Se, Cu, Pb, Zn, Fe, Co, Ni, Mn, Cr and Cd in water

Sodium diethyldithiocarbamate in the presence of a weak oxidizing agent is used as a co-precipitative agent for the pre-concentration of Se, Cu, Pb, Zn, Fe, Co, Ni, Mn, Cr and Cd. A procedure was developed for ICP-AES determination of these elements after pre-concentration in river and waste water (an enrichment factor of 40). The recovery of all the elements tested for was more than 98%. The limits of determination (mg l⁻¹) (10 S.D. blank) are 0.001 (Cu, Co, Cr, Mn), 0.0007 (Zn, Cd), 0.003 (Se), 0.004 (Fe), 0.007 (Ni), and 0.01 (Pb).     

Element content and element correlations in Chinese human liver

The amounts of the 19 elements As, Br, Ca, Cd, Ce, Co, Cr, Cs, Fe, K, La, Mo, Na, Rb, Sb, Sc, Se, Sm, and Zn in 92 lyophilized autopsy human liver samples from normal subjects have been analyzed by instrumental neutron-activation analysis (INAA). For intercomparison and quality control ten samples were independently analyzed in two institutes, the Institute of High Energy Physics in China and the Joef Stefan Institute in Slovenia. Most of the element contents determined by the two institutes were in quite good agreement, even though different experimental conditions were applied, indicating the reliability of the analytical results. Analysis of the chemical species of mercury present in the ten liver samples was also performed in Slovenia. Possible differences between the element content of male and female liver samples were studied by means of Students t-test, but significant differences were found only for Ce, Co, Fe, La, Mo, and Zn. The results obtained were also compared with those reported from other areas of the world; no appreciable differences were observed. Correlation among the various elements in the human liver samples was studied using multivariate statistics. It was found that there was relatively close correlation between some elements, for example As–Fe, Ca–Fe, Cd–Co, Cd–Zn, Mo–Zn, Co–Se, Cs–Rb, Br–Rb, Sc–Sm, La–Sm, La–Ce, etc.; these correlations could be rationally explained by the similarity of the electronic structures of the elements and/or their physiological functions in the human body.     

Instrumental neutron activation analysis of 23 individual food articles from a high altitude region

Twenty-three individual food items commonly consumed in a high altitude region (Kashmir) have been investigated using instrumental neutron activation analysis. The concentration of Ca, Cl, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Na, Se, Sn, and Zn is reported for these food articles. For quality assurance of our data, IAEA and NIST standard reference materials have also been studied. The dietary intake of these elements was calculated in accordance with the weekly food selection habits of the residents of this area. The dietary contribution of most of these elements was found to be in agreement to the RDA/ESadi levels. The purpose was to design a database of essential elements for this area and to study the adequacy levels of these elements in different dietary items. Fairly adequate intake of Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Se, Sn, and Zn through these foodstuffs is reported, whereas, lower intakes through these items were found for Cl, K, and Na.