Substoichiometric and non-destructive determination of trace impurities in high-purity optical glasses by neutron activation analysis

A method of radioactivation analysis has been developed for the determination of 17 elements as impurities in high-purity optical glasses. The substoichiometric extraction of platinum with dithizone was studied and a simple procedure was proposed for the determination of platinum. Copper and manganese were also determined substoichiometrically by the extractions with dithizone and with thenoyltrifluoracetone, respectively. The non-destructive γ-ray spectrometry using a Ge(Li) detector has been applied for the determination of the other 14 elements (Ag, Co, Cr, Eu, Fe, Ir, Sc, Zn, Cs, Hf, Rb, Sb, Ta and Tb). Impurity elements at the ppb level were analysed by the proposed method and it is shown that the method is reliable for the determination of trace impurities in high-purity optical glasses.     

Instrumental and radiochemical neutron activation analysis techniques for protein bound trace metals in human serum

Gel filtration and neutron activation analysis methods were combined in work aimed at the development of methods for the determination of metals firmly bound to protein in human blood serum. The values obtained are semiquantative. A purely instrumental technique afforded data on Cu, Fe, Zn, Al and Mn but values for the latter two only were determined since Cu, Fe and Zn are already well known. The concentrations for Al and Mn were found to be 300 ppb and 0.4 ppb, respectively. Despite the high resolution of Ge(Li) detectors, no other metals were found. For the determination of any others, radiochemical separations are necessary and were used to obtain data on the following elements: As 3 ppb, Ag 3 ppb, Au 0.003 ppb, Cr 1 ppb, Sb 1 ppb, Co, Cd, Mo and Sn could not be detected and upper limits were estimated to be 0.1 ppb, 2 ppb, 2 ppb, and 1 ppb, respectively.     

Multielement neutron activation analysis of biological materials using chemical group separation and Ge(Li) gamma spectrometry

Neutron activation analysis (NAA) for the determination of some trace elements in biological materials is described. The method presented permits the simple and rapid determination of Se, Ag, Au, Sb, Pt (via¹⁹⁹Au), Hg, Co, Ni (via⁵⁸Co), Fe, Zn, Mo, Sn, Cr, Cd, Cu and As after radiochemical separation from Na, K, Cs, Rb and partially Br. For this purpose, postirradiation separation by extraction with mercury or zinc amalgam was used. Separation of gold by extraction with ethyl acetate or by precipitation with dimethylglyoxime was applied for the determination of gold and platinum in biological materials.     

Determination of nickel,gold and silver in gallium arsenide by radioactivation analysis based on the quantitative isotope dilution principle

A method of radioactivation analysis has been developed for the determination of Ni, Au and Ag impurities in gallium arsenide. The separation and substoichiometric extraction of these elements were studied and analytical procedures are suggested for their determination. All components are separated by suitable procedures and determined by substoichiometric methods. Ni is extracted as diethyldithiocarbamate into toluene, Au as a complex of rhodamine-B in chloroform, and Ag as dithizonate in carbon tetrachloride. The contents of Ni, Au and Ag in a gallium arsenide crystal with a carrier concentration of 1.8·10¹⁶/cm³ were 0.05–0.08, 0.006–0.008 and 0.002–0.005 ppm, respectively.     

Grundlagen zur halbquantitativen Bestimmung von zwanzig Elementen in der Lasermikrospektralanalyse

Zusammenfassung Für die folgenden 20 Elemente wurden die Grundlagen für eine halbquantitative Konzentrationsbestimmung mit Hilfe des Laser-Mikrospektralanalysators ermittelt, und zwar differenziert für Untersuchungen an oxidischen und an metallischen Materialien: Mg, Al, Si, Cr, Mn, Co, Ni, Cu, Zn, Ga, Ge, Pd, Ag, Cd, In, Sn, Sb, Pb, Bi, Fe bzw. Au.

---

Principles of semi-quantitative determination of 20 elements by laser-microspectroscopy

The principles for the determination of the following 20 elements by Laser-microspectroscopy have been investigated separately for oxidic and metallic materials: Mg, Al, Si, Cr, Mn, Co, Ni, Cu, Zn, Ga, Ge, Pd, Ag, Cd, In, Sn, Sb, Pb, Bi, Fe resp. Au.

     

Neutron activation analysis of laundry dryer lint

The concentrations of 22 elements in 10 laundry dryer lint samples were determined by computerized systematic instrumental absolute neutron activation analysis. The mean concentrations (and their standard deviations) of Al, Ag, Au, Br, Ca, Cl, Co, Cr, Cu, Fe, I, K, Mg, Mn, Na, Sb, Sc, Se, Ti, U, V and Zn were equal to 966(633), 2.4(0.9), 0.13(0.07), 19(13), 3725(1262), 566(153), 1.0(0.4), 27(18), 62(32), 471(146), 1.3(1), 221(78), 1102(384), 6(2), 433(216), 14(14), 0.07(0.06), 9(5), 291(125), 0.5(0.3), 1.1(0.6) and 90(141) ppm respectively. They were compared with the mean concentrations in the Earth's crust. The concentrations of Ag, Au, Sb and Se were found to be significantly (>10) enriched in the lint. Their origin was tentatively established (except for Sb). The purpose of this work was to determine the background levels for different elements in this material, in order to use it for environmental screening for these elements.     

Determination of trace elements of Egyptian crops by neutron activation analysis

Multielemental neutron activation analysis was used for the determination of Al, As, Au, Br, Ca, Cd, Co, Cr, Cu, Fe, La, Mn, Mo, Sb, Se, W and Zn in African tea, and lady's fingers (Malvaceae Family), ginger (Zingiperaceae Family), canella bark (Laureceae Family), black pepper (Piperaceae Family), cucumber seeds and vegetable marrow seeds (Cucurbitaceae Family), tomatos seed (Solanaceae Family), safflower seeds (Compositae Family), jew's mallow seeds (Tiliaceae Family) and sesame (Pedaliaceae Family). Trace elements determination was made to the analysis of destructive (using super pure nitric acid and adsorbing the metal-APDC and metal-Dz complexes on activated charcoal) and nondestructive (dry seeds) samples. The method is simple, precise and sensitive for the determination of microamounts of the elements (ppm to ppb).     

Instrumental neutron activation analysis of brewer's yeast

Instrumental neutron activation was used for the determination of 23 trace and minor elements in 4 different samples of brewer's yeast. Detection limits for these elements vary from 2 ppb to 100 ppm. The following average concentrations were found (ppm, dry weight): Al 597, Br 0.36, Cl 1473, Co 0.21, Cu 19, Fe 285, K 16 400, Mg 1355, Mn 8.4, Na 2330, Rb 19, Sb 0.053, Se 1.2, V 2.2 and Zn 80. NBS standard 1569 was also analyzed and the following concentrations (in ppm) were measured: Al 2300, Br 0.65, Ce 0.23, Cl 460, Co 0.26, Cr 2.12, Cu 11, Fe 707, Gd 7.1, Hf 0.13, K 15 500, Mg 1780, Mn 7, Na 510, Rb 16, Sb 0.075, Sc 0.18, Se 0.92, Th 3.7, Ti 38, U 0.49, V 4.1 and Zn 70.     

Investigation of silicon dioxide films by neutron activation analysis and autoradiography

Investigations of insulating silicon dioxide films formed on silicon epitaxial layers are reported. Activation analysis and surface autoradiography were used to determine the concentration distribution and precipitation of contaminants in the internal part of the films and on the surfaces. The aim of this work was to study the origin of the contaminants by sampling each technological product following thermal oxidation, doped oxide deposition, heating and metallizing. Under the given conditions the following detection limits of impurities could be obtained in silicon dioxide films: Na=80 ppb, Sb=100 ppb, Cu=20 ppb and Au=5 ppb.     

Determinations de traces dans les semi-conducteurs par activation neutronique

Résumé On décrit la détermination de traces dans le germanium, le silicium et le sélénium. En appliquant des techniques gamma spectrométriques, précédées ou non de séparations chimiques il est possible de doser les éléments suivants dans (1) germanium: As, Cu, Au, Ga, Zn, Hg, Cr, Sn, Sb, Co, In, Ni, Ir, Se, Sc, Ag, Ta, Hf et U; (2) silicium: P, Au, Sb, Ga, Fe, K, Cr, Mo, Sn, As, Co, In, Zn, Cu, W, Ta, Na, Eu, Sm, La, Sc et T1; (3) sélénium: Cl, Br, I, P, S, Te, Na, K, Cr, Fe, Co, Cu, Zn, Ga, Sc, Ag, Cd, La, W, Au et Tl. Les concentrations et ou limites de détections varient de quelques parties par million à 10⁻³ parties par milliard.     

Determination of impurities in titanium and titanium dioxide by neutron activation analysis : Simultaneous determination of 16 trace elements in titanium

The most important metallic impurities in titanium which give long-lived isotopes on neutron irradiation can be determined by a rapid anion-exchanged seperation of Ti, Sc, Cr, Na and Ag, after which the resin, containing most of the impurities, is counted on a high-resolution Ge(Li) γ-spectrometer. Cu, W, As, Ga, Au, Sn, Fe, Zn, Co, Ta, Mo and Ni can be determined in one measurement, while Na, Cr and Ag can be determined after an additional separation from the Sc isotopes, the major activities originating from the titanium on neutron irradiation. Three different samples were analysed five times, and the reproducibility of the results was good.     

天然杂质对闪锌矿电子结构和半导体性质的影响

采用密度泛函理论系统研究了分别含有十四种天然杂质的闪锌矿的电子结构,并讨论了这十四种杂质对闪锌矿半导体性质的影响.研究结果表明,锰、铁、钴、镍、铜、镉、汞、银、铅、锑杂质的存在使闪锌矿的带隙变窄,导致吸收带边增大.除了镉和汞杂质外,其余杂质的存在均导致费米能级向高能级方向移动,并且在闪锌矿禁带中产生了杂质能级.铁、镓、锗、铟、锡、锑杂质使闪锌矿的半导体类型由p型变为n型;而锰、钴、镍、铜、镉、汞、银、铅杂质对闪锌矿的半导体类型没有影响.铜杂质使闪锌矿由直接带隙变为间接带隙半导体.     

Instrumental neutron activation analysis of a sulfide ore and some ore benefication products

Samples of a pyritic lead-zinc ore and some benefication products were examined by instrumental activation analysis using Ge(Li) gamma-spectrometry. The following elements were determined using thermal neutron activation: Sc, Cr, Co, Zn, As, Se, Ag, Sb, Ir, Au and Th. The technique is especially favourable for the determination of cobalt, arsenic, antimony and gold, but selenium, silver and thorium can also be determined in most fractions. Activation with epithermal neutrons will improve conditions for the determination of As, Sb, Se, Ag, Au and Th.     

Neutron activation as a routine method for the determination of trace elements in water

By freeze-drying the following elements can be determined in natural water except sea water: Au, Ba, Br, Ca, Ce, Co, Cr, Eu, Fe, K, La, Mo, Na, Sb, Sc, Se, U, Zn. Some problems may arise with respect to As and Hg. Cu, Cd and Ni can only be determined if present in high concentrations. Separation by adsorption on charcoal in presence of complexing agents gives yields between 75 and 100% for the following elements in sea water: Ag, Au, Cd, Ce, Co, Cr, Eu, Fe, Hg, La, Mo, Sc, Se, U, Zn (As 67%, Sb 56%). Activation or use of labelled ions and study of exchange give information about mobility of trace elements in suspended matter.     

Determination of impurities in semiconductor grade silicon by instrumental neutron activation analysis

Instrumental neutron activation analysis has been applied to semiconductor grade silicon to study the concentration levels of impurity elements, the contamination during the single crystal growing process, and the vertical and radial distributions of impurities, along with the decontamination effect in the analysis. Twenty elements of Au, Br, As, W, Cr, Co, Na, Eu, La, Se, Zn, U, Th, Hf, Fe, Sb, Ag, Ce, Tb and Ta have been analyzed in p- and n-type wafers, single crystals and a polycrystal by a single comparator method using two comparators of gold and cobalt. Considerable surface contamination has been found and could be removed by etching the surface with nitric and hydrofluoric acid before and after irradiation. The impurity concentration has been found to be generally increased in the process of single crystal growth. The vertical and radial distributions of impurities have revealed that some impurity elements were more concentrated in the top region of a single crystal rod than in the middle region, and that Br, Cr, La, Eu and Sb were enriched in the central region and As, U and Fe in the outer region.     

Determination of impurities in high-purity niobium(V) oxide by high-resolution continuum source graphite furnace atomic absorption spectrometry after sorption preconcentration

Method of sorption–atomic-absorption determination of Co, Cr, Cu, Fe, Mn, and Ni in samples of high-purity Nb₂O₅ with heterochain S,N-containing sorbents was developed. The method is based on the sorption preconcentration of trace impurities followed by their determination by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). Selectivity of three original inhouse synthesized S,N-containing heterochain sorbents was studied. The recoveries of Co, Cr, Cu, Fe, Mn, and Ni using heterochain sorbents OKS, MTH, and GLSH were 100, 80, and 76%, correspondingly. Sorbent “OKS”, which provided the quantitative recovery of trace impurities, was chosen for further research. The sorption conditions for chloride solutions of different acidities (0.1–3 M HCl) were studied and optimized. Using the conditions established for the sorption and HR CS GFAAS analysis, trace Co, Cr, Cu, Fe, Mn, and Ni were determined in high purity Nb₂O₅ with a relative error less than 5%. The trueness control of the obtained results is confirmed by the “added–found” method. The developed method allows us to determine concentrations of analytes: 0.02–0.20 ppm Co, 2.0–3.3 ppm Cr, 0.2–1.5 ppm Cu, 6.0–21.0 ppm Fe, 0.6–0.8 ppm Mn, and 2.8–3.5 ppm Ni. The proposed methodology can be successfully extended to the determination of various trace elements in other high-purity inorganic materials.     

Solvent extraction of metal xanthates

The solvent extraction of metal xanthates is reviewed with emphasis on the characteristics and analytical uses of ethyl xanthate complexes. Elements reviewed include As, Sb, Bi, Cd, Co, Cu. Cr, Ga, Au, In, Fe, Pb, Mn, Hg, Mo, Ni, Pd, Pt, Re, Ag, Se, Te, Tc, Tl, Sn, U, V and Zn.     

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.     

Compositional Studies of Ancient Copper from Romanian Territories

Ancient copper objects from Romanian territories have been analyzed by neutron activation analysis. A series of elements is determined: Au, Ag, As, Co, Cr, Fe, Hg, Ni, Zn, Sb, Sc, Se, Sn. Using mathematical dendograms some classifications and correlation have been established.     

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.

---

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.

---

---

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

---

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