The direct micro determination of oxygen in organic material

A procedure is described in which interferences caused by hydrogen and sulphur are eliminated. These occur when petroleum hydrocarbons or sulphur containing materials are analysed. Copper oxide, in conjunction with the gravimetric determination of carbon dioxide, has been found preferable to the iodine pentoxide procedure. The replacement of iodine pentoxide by copper oxide has also simplified the maintenance of the apparatus without any loss of applicability to organic compounds in general. Activated copper is used to absorb sulphur compounds. Details of the modified procedure are included.     

Decomposition of organic matter with molten alkali: determination of arsenic and antimony in organic compounds

Decomposition of organic matter with molten alkali has been examined as a method of opening out organic matrices for elemental detection and/or determination. The fusion product is readily soluble. Arsenic and antimony in organic compounds can be determined iodimetrically after mineralization by this fusion method.     

Organic reagents in inverse voltammetry: A review

Summary A review is presented on electrochemical and adsorption processes for the preconcentration of inorganic ions and organic compounds by the use of organic reagents forming with the elements to be determined insoluble compounds on the electrode surface or surface-active complexes. Quantitative determinations are based on the electrochemical oxidation or reduction of the concentrate formed on the electrode. The processes examined comprise inverse voltammetry of variable-valence ions and adsorption inverse voltammetry. Examples are given of the use of organic reagents in the inverse voltammetry of antimony, iodine, cobalt, nickel, cerium, aluminium, vanadium and molybdenum.

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Organische Reagentien in der Iversen Voltammetrie. Ein Überblick

Zusammenfassung Ein Überblick wird gegeben über elektrochemische und Adsorptionsverfahren zur Anreicherung anorganischer Ionen und organischer Verbindungen mit Hilfe organischer Reagentien, die mit den zu bestimmenden Elementen unlösliche Verbindungen auf der Elektrodenoberfläche oder oberflächenaktive Komplexe bilden. Quantitative Messungen beruhen auf der elektrochemischen Oxidation oder Reduktion des an der Elektrode gebildeten Konzentrates. Die behandelten Verfahren umfassen die Inverse Voltammetrie von Ionen variabler Wertigkeit sowie die Inverse Adsorptionsvoltammetrie. Anwendungsbeispiele für die Verwendung organischer Reagentien werden gegeben für Antimon, Iod, Cobalt, Nickel, Cer, Aluminium, Vanadium und Molybdän.

     

Multi-element analysis of blood for trace metals by neutron activation analysis

Fourteen elements can be rapidly determined in whole blood by the neutron activation analysis procedure described. Three of these (Ag, Cl, Se) are measured after a 10-s irradiation and eleven others (Al, Ba, Br, Ca, Cu, I, Mg, Mn, Mo, Rb, V) are determined by a 180-s irradiation of a 1-cm³ sample of whole blood after destruction of organic matter and removal of sodium by hydrated antimony pentoxide. A further 13 elements (As, Au, Co, Cr, Cs, Fe, Hg, K, Na, Ni, Sb, Sc, Zn) are determined after overnight irradiation in the SLOWPOKE reactor.     

Indirect radiotracer study of the adsorption of organic compounds at platinized platinum electrodes

The possibility of the use of an indirect radiotracer method for the study of the adsorption of organic species has been discussed. It has been shown that by study of the adsorption of Cl-36 labelled chloride ions in the presence of organic species such as maleic, benzoic and m-nitrobenzoic acids there is a possibility of obtaining information concerning the adsorption of the latter compounds. Change in the adsorption behaviour of organic species connected with their electroreduction were detected and followed by indirect tracer measurements. In the light of the experimental results, some mechanistic aspects of the reduction of aromatic nitro compounds are discussed.     

Multielemental analysis of Brazilian milk powder and bread samples by neutron activation

The concentrations of Na, Cl, Mn, Br, Fe, Zn, Rb, Sb, Sc, Cr, Al and Mg were determined in some types of bread and in some brands of milk powder consumed in the city of São Paulo (SP—Brasil), by instrumental neutron activation analysis. Radiochemical separations were carried out by means of retention of²⁴Na on hydrated antimony pentoxide (HAP) from a 8N HCl solution, after digestion of the organic matter. It was possible in this way to determine the radioisotopes⁶⁴Cu,^69mZn and¹⁴⁰La in the effluent solution. The detection limits of the trace elements analyzed in bread and milk powder samples were determined using the Currie and Girardi criterions.From a dissertation submitted by V. A. MAIHARA to the University of São Paulo in partial fullfillment of the requirements for a Master of Science Degree in Nuclear Technology.     

分子连接性指数与溶液吸附自由能的相关性

测定了硅胶自四氯化碳中吸附脂肪醇及活性炭自水中吸附芳香化合物的吸附等温线, 等温线均可用Langmuir方程描述。利用Langmuir参数计算了各体系的吸附标准自由能变化。计算了各种吸附质的分子连接性指数。各种分子的分子连接性指数与吸附标准自由能变化间有相关性, 并给出了相关方程, 同时作了初步的讨论。     

Radiochemical separations by adsorption on some oxides of groups IVB and VB

The interactions between titanium dioxide, niobium pentoxide and tantalum pentoxide and 55 elements have been studied by batch experiments in nitric acid. The variation of the distribution ccefficients with nitric acid concentration is presented and discussed. The adsorption mechanism for some ions has also been investigated. Column experiments have been carried out to check the practical use of the investigated oxides in radiochemical separations. A^99mTc generator based on the use of TiO₂ is also presented.     

Determination of short-lived activation products in neutron-irradiated sodium through application of hydrated antimony pentoxide

A method for the determination of short-lived activation products in neutron-irradiated sodium is described. It is based on hydrolysis of sodium with methanol, separation of Na⁺ with specially prepared antimony pentoxide (HAP) possessing very high selectivity and capacity, and subsequent gamma-spectroscopic measurement of the activation products.     

Fr and Ra fixation on some inorganic sorbents or mixed composite ion exchangers

Zinc and nickel hexacyanoferrates (II) present a high affinity for²²³Fr and no retention for²²³Ra in hydrochloric acid solutions with concentrations greater than 0.5N. Hydrated antimony pentoxide is the best sorbent for²²³Ra. Incorporated in a composite exchanger, it could be used for decontamination purposes.     

Determination of some toxic trace metals in Nigerian river and harbor water samples by neutron activation analysis

The determination of As, Cd, Cr, Hg, Mn, Mo, Ni, Sb, and Se in two Nigerian rivers and two Nigerian harbor waters is described. The water samples were preconcentrated by both evaporation at room temperature and freeze evaporation under reduced pressure. Postirradiation chemical separation of sodium, using hydrated antimony pentoxide (HAP) in 6M HCl, and of bromine, by oxidation with KMnO₄ and subsequent removal by extraction with CHCl₃, was employed. The measured concentrations of these elements in some water samples, which are relatively high, can be attributed to local pollution.     

Inverse voltammetry of antimony with triphenylmethane dyes

A method is suggested for the determination of traces of antimony by inverse voltammetry of the solid phases formed with triphenylmethane dyes (Crystal Violet, Methyl Violet and Malachite Green) as the precipitants. The authors have studied the effect of concentration, adsorption and oxidation of the triphenylmethane dyes, potential and time of pre-electrolysis, and concentration of antimony(III) and some other elements on the polarogram shape and stripping current. A method for determining antimony traces in chromic salts is described as an example.     

In Process Citation

The isotherms for adsorption of some organic molecules on asbestos fibres have been determined by gas chromatography. The results show that the adsorption mechanism lies somewhere between physisorption and chemisorption. The degree of adsorption at a given temperature, for the compounds studied, is toluene > tetrahydrofuran > benzene > dichlorométhane.     

Determination of selected trace metals in scallops by flame atomic absorption spectrometry after removal of sodium on hydrated antimony pentoxide

Hydrated antimony pentoxide is used to remove sodium ion for the determination of trace metals in scallop specimens of Plactopecten magellanicus. The concentrations of Cd, Cr, Co, Cu, Au, Fe, Pb, Mn, Hg, Ni, Ag and Zn were determined in the samples and in a standard reference material. This method yields improved detection limits with simple apparatus.     

Electronic structure and luminescent properties of antimony(III) complex compounds with nitrogen containing outer-sphere organic cations

X-Ray photoelectron (XPS) and luminescent spectroscopy have been used to investigate complex compounds of antimony(III) halides with nitrogen containing organic bases. Inequality of bonds of amine and imine groups was found by XPS to disappear when complexes of antimony(III) with N,N′-diphenylguanidine (Dphg) were formed. The appearance of N1s symmetric line when transiting from Dphg to the cation N,N′-diphenylguanidine ( Dphg⁺) in complex compounds of antimony(III) testifies to this. The study performed demonstrates that electron density increment on the antimony(III) central atom (complexing agent) results in the bathochromic shift ³P₁ → ¹ S ₀ of the luminescence band of antimony(III) ion.     

吸附树脂对微污染水中有机污染物的吸附研究

以活性炭作为参照,从静态和动态吸附角度,利用3种吸附树脂对微污染水中代表性污染物氯仿、三氯乙烯、2,4-二氯苯酚和腐殖酸进行了吸附去除效果研究。结果表明,吸附树脂对水溶液中有机物吸附去除具有较好的效果,但仍然存在进一步提高吸附容量的问题。     

在玻璃的TiO2涂膜上有机物分子的吸附及光催化分解对水接触角的影响

研究了有机物分子在玻璃的TiO₂ 和WO₃/TiO₂ 复合物涂膜上的吸附及光催化分解对水接触角的影响.结果表明:有机物在空白玻璃及其膜的表面的吸附为不可逆化学吸附,WO₃/TiO₂ 复合物膜可钝化玻璃表面对大气污染物分子的吸附能力并具有较好的光催化活性.     

Modeling of the adsorption of organic compounds on polymeric nanofiltration membranes in solutions containing two compounds.

The adsorption of organic compounds in aqueous solution on polymeric nanofiltration membranes is studied; this process is one of the most important fouling mechanisms influencing the flux and retention behavior of nanofiltration membranes. It is shown that the adsorption of dissolved organic compounds on polymeric nanofiltration membranes is comparable to that on activated carbon. Freundlich and Langmuir isotherms are used to describe the relation between the adsorbed mass on the membrane and the equilibrium concentration of the organic compound in a single-compound solution. Based on these results, three models for the adsorption of solutions containing several compounds [i.e., the simple competitive adsorption model (SCAM), the model of Jain-Snoeyinck, and the model of Butler-Ockrent] were used to predict the adsorption behavior of an organic compound in an aqueous solution containing two compounds. The results of the three models were compared to experimental observations. It is shown that the SCAM allows a good prediction of the adsorption behavior.     

Mild One-Pot Deoximation and Conjugate Reduction of α, β-Unsaturated Ketoximes with Hydrosilane and I2O5

The organic chemistry of polyvalent iodine compounds has experienced an unprecedented development during the last decade of 20th century.[1,2] On the other hand, despite its extensive use in industry, I2O5 (iodine pentoxide, IP) has rarely been employed in organic synthesis except as an alternative to iodoxybenzoic acid (IBX) for the dehydrogenation of aldehydes and ketones.[3] Generally, pentavalent iodine reagents, such as IBX and Dess-Martin periodinane (DMP)were used as mild and selective oxidants for oxidation of alcohols[1,2] and dehydrogenation of carbonyl compounds.[3] We wish to report herein that IP can serve as a mild and efficient reagent for the oxidative cleavage of oximes to aldehydes and ketones (Eq. 1). Most interestingly, IP can also activate hydrosilanes for reduction of alkenes. Hence, simultaneous deoximation and conjugate reduction of α,β-unsaturated ketoximes can be achieved by using IP and phenyldimethylsilane (Eq. 2).