On the loss of cadmium, antimony and silver during dry ashing of biological material

Summary The loss of cadmium, antimony and silver during dry ashing of marine weeds, mussels and shrimps was studied with the aid of radioactive tracers. Except for antimony all biological material was labelled by uptake of the radioactive tracers by the organisms while still alive. At an ashing temperature of 500° C and below no significant loss by volatilization of these elements occurs. The results obtained at higher temperatures with cadmium show that the behaviour of this element may depend on the composition of the organic material. Retention on the wall of quartz crucibles did not cause serious losses.

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Über den Verlust an Cadmium, Antimon und Silber bei der Trockenveraschung von biologischem Material

Zusammenfassung Mit Hilfe radioaktiver Tracer wurden die Verluste an Cadmium, Antimon und Silber bei der Trockenveraschung von Seetang, Muscheln und Krabben untersucht. Mit Ausnahme von Antimon wurden alle Materialien mit den Tracern durch Aufnahme im lebenden Zustand markiert. Bei Veraschungstemperaturen von 500° C und darunter konnten keine signifikanten Verluste durch Verflüchtigung der Elemente festgestellt werden. Das Verhalten von Cadmium bei höheren Temperaturen kann von der Zusammensetzung des organischen Materials abhängen. Verluste durch Haften an der Wand des Quarztiegels waren unbedeutend.

     

THE PARAMETER KERNELS FOR THE LINEAR INVERSION OF THE FREE OSCILLATION OF THE EARTH (Ⅰ)

In the linear inversion of the radial variation of the parameters of the Earth by usingthe observed frequencies of various normal modes of free oscillation of the earth, it is neces-sary to know the values of the kernels of the parameters ρ, μ and λ. This paper describesthe methods of the derivation of the formulas of these kernels. This is the first part of thepaper in which only the toroidal oscillations are considered. They are much simpler thanthose of the spheroidal ones, that we will consider in the second part of the paper. The data of the two types of oscillations are equally important in the solution of theinversion problem, and should be employed simultaneously, and we know that the toroidaloscillations are much simpler than the spheroidal ones, it seems wise to divide the whole programof the inversion problem into steps: first, by employing the toroidal data to correct the twoparameters ρ and μ in the mantle, then by using the spheroidal data to correct the remain-ing parameters, i.e. th     

Effect of the polyethylene confinement and topology on its crystallisation within semicrystalline ABC triblock copolymers

The isothermal crystallisation behaviour of the polyethylene block within polystyrene-b-polyethylene-b-poly(ε-caprolactone), SEC, triblock copolymers was studied by differential scanning calorimetry. The morphology was observed by transmission electron microscopy. Melting scans after isothermal crystallisation performed at different times were employed to determine the crystallisation kinetics one step at a time (“isothermal step crystallisation”). Double melting endotherms were observed after isothermal crystallisation and they were interpreted as a result of the melting of two lamellar populations. These arise from the intrinsic short chain branching distribution within the hydrogenated polybutadiene chains that conform the PE blocks and from their location within the copolymer microdomains. The Hoffman-Weeks procedure failed to yield reasonable values for the equilibrium melting point of the PE blocks as a result of the distribution of linear sequences present in these blocks. The results indicate that as the degree of PE confinement increases the Avrami index decreases to values that are even lower than 1, a result that can be explained by the nature of the homogeneous nucleation process that is in between sporadic and instantaneous.     

Determination of rare earth impurities in high purity uranium by isotope dilution analysis

Summary An isotope dilution method for the determination of rare earth impurities in uranium has been developed and Ce, Nd, Sm, Eu and Gd have been determined in uranium oxide samples. The method involves isotopic dilution with enriched isotopes of the rare earths being measured, followed by the separation of rare earths from uranium. A mass spectrometer with thermionic source was used to determine the relative isotopic abundances in each of these rare earths. All these five elements were analysed selectively by preferential evaporation technique. Trace concentrations down to parts per billion range can be measured with good sensitivity and accuracy.

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Bestimmung von Verunreinigungen an Seltenen Erden in hochreinem Uran durch Isotopenverdünnungsanalyse

Zusammenfassung Eine Isotopenverdünnungsmethode wurde ausgearbeitet zur Bestimmung von Ce, Nd, Sm, Eu und Gd in Uranoxidproben. Das Verfahren umfaßt isotopische Verdünnung mit angereicherten Isotopen der zu bestimmenden Elemente und nachfolgende Abtrennung der Seltenen Erden von Uran. Die relativen Isotopenhäufigkeiten wurden mit Hilfe eines Massenspektrometers mit thermischer Ionenquelle bestimmt. Alle fünf Elemente wurden durch selektive Verdampfung analysiert. Spurenkonzentrationen bis herab zum ppb-Bereich konnten mit guter Empfindlichkeit und Genauigkeit erfaßt werden.

     

一种新型的表面声波阻抗传感器及其在液相体系中的应用

一种新型的表面声波阻抗传感器及其在液相体系中的应用姚守拙，陈康，刘德忠，聂利华（湖南大学化学化工系，长沙，４１００８２）关键词表面声波，阻抗传感器，液相应用表面声波传感器（ＳＡＷＳ）具有较高的灵敏度和检测精度，已广泛应用于气体微量组分分析、色谱检测和...     

Enantioselectivity of 6-O-alkyldimethylsilyl-2,3-di-O-methyl-β-cyclodextrins as chiral stationary phases in capillary GC

Summary Clenbuterol has been determined in urine by solidphase extraction on a C₁₈ cartridge, diazotization of the eluate with nitrite, coupling of the diazonium ion with 1-(naphthyl)ethylenediamine, and separation of the azo dye formed by HPLC with a C₁₈ column and a micellar mobile phase containing 0.1 M sodium dodecyl sulphate, 12%n-butanol and 0.05 M citrate buffer, pH 3. Recoveries higher than 90% were obtained by mixing the samples with a 20% 0.2 M NaOH before extraction. Limits of detection of 51 and 6.7 ng L⁻¹ were obtained with spectrophotometric and thermal lens spectrometric detection, respectively; respective repeatabilities were 3.1% (5 μg mL⁻¹) and 5.6% (0.16 μg mL⁻¹).     

A simple procedure for the chromatographic isolation and determination of prostaglandins from human seminal plasma

Summary A relatively simple procedure for the isolation and determination of the prostaglandins present in human seminal fluid is described. It involves preliminary chromatographic purification of these compounds from the major non-prostaglandin impurities followed by their total elution in one solvent (one-step elution). The prostaglandins thus obtained were almost free from other lipids and were further resolved into prostaglandin-groups and individual prostaglandins by repeated thin-layer chromatography. Data are also presented for prostaglandin contents of fresh semen samples from five individuals and results compared with those from the stored samples.

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Einfaches Verfahren zur chromatographischen Isolierung und Bestimmung von Prostaglandinen aus menschlichem Sperma

Zusammenfassung Das Verfahren umfaßt eine chromatographische Abtrennung der Verbindungen von den hauptsächlichsten Verunreinigungen und die Gesamtelution mit einem Lösungsmittel. Die von anderen Lipiden fast völlig freien Prostaglandine werden durch wiederholte Dünnschicht-Chromatographie in Gruppen und Einzelverbindungen getrennt. Werte werden angegeben über die Prostaglandingehalte von frischem im Vergleich zu gelagertem Sperma.

     

Analysis of 19-norandrosterone in human urine by gas chromatography–isotope-dilution mass spectrometry: method adopted by LGC for participation in the Comité Consultatif pour la Quantité de Matière (CCQM) Pilot Study P68

The method used at LGC for analysis of “total” 19-norandrosterone (19-norandrosterone glucuronide plus “free” 19-norandrosterone) in urine for the Comité Consultatif pour la Quantité de Matière Pilot Study (CCQM-P68) is described. The analytical method used was a modified version of the method developed at the National Measurement Institute of Australia, which used a hydrolysis and derivatisation procedure first described by the German Sports University. This method is routinely used by World Anti-Doping Agency-accredited laboratories for sports drug testing. The main modifications made to the method were the use of 19-norandrosterone glucuronide as a calibration standard and 19-norandrosterone glucuronide-d4 as an isotopically labelled internal standard, and the use of a bench-top quadrupole gas chromatograph–mass spectrometer. The results produced by LGC (2.14 ± 0.15 ng g⁻¹ expanded uncertainty, coverage factor k = 2) were in excellent agreement with those from other participating national metrology institutes and thus further validates the exact-matching isotope-dilution mass spectrometric procedures used at LGC for a wide range of reference measurement applications, including measurement of ng g⁻¹ levels of steroids in a biological matrix.     

Reaction of η5-cyclopentadienylbis(triphenylphosphine)cobalt(I) with alkadiynes. Preparation and reactions of bicyclic cobalt metallocycles and a stable trimethylsilyl-substituted mono-complexed alkadiyne. Comments on the mechanism of cobalt-catalyzed alkyne cooligomerization

Reactions of η⁵-cyclopentadienylbis(triphenylphosphine)cobalt(I) (5) with several 2,n-alkadiynes (2) were investigated. Each of these reactions leads initially to a material in which one of the acetylene functional groups is π-coordinated to cobalt; this complex then undergoes conversion to a metallocycle. In cases where the two acetylene functions are connected by three- and four-carbon bridges (2b, 2c), metallocycles formed by intramolecular reaction of two acetylene functions in the same molecule may be isolated. In cases where the acetylene functions are joined by larger or smaller bridges, the reactions are more complex, and both inter- and intramolecular metallocycles are formed. Reactions of 5 with 1,8-bis(trimethylsilyl)-1,7-octadiyne (16) gives an isolable crystalline mono-acetylene complex (17), this material is stable in the solid state but undergoes conversion to metallocycle (18) in benzene solution. The relationship of these results to the mechanism of the CpCo(CO)₂-catalyzed benzocycloalkene synthesis is discussed; it is suggested that intramolecular metallocycles are intermediates in reactions leading to benzocyclopentanes and -cyclohexenes, but intermolecular metallocycles are probably involved in reactions leading to benzocyclobutenes.