Micro Determination of Ammonia by a Kinetic Spectrophotometric Method

 A simple and sensitive kinetic spectrophotometric method is described for the determination of micro amounts of ammonia. The method is based on the inhibiting effect of ammonia on the oxidation rate of aqua ethylenediamine-tetraacetate chromium(III) [Cr(HEDTA)(H₂O)] with N-bromo succinimide (NBS) to yield chromium(VI). The reaction was followed spectrophotometrically by measuring the rate of change in absorbance with time at 365 nm, which is the maximum absorption wavelength of chromium(VI). Using the recommended procedure, ammonia can be determined up to 153 μg ml⁻¹ with a linear calibration graph and a detection limit of 0.09 μg ml⁻¹. The method was successfully applied to the determination of ammonia in waste water samples. Recovery experiments for the analyzed samples were 97–100% with relative standard deviation, Sr (%) of ≤ 2.9% indicating high accuracy and precision of the proposed method. The interference of various cations and anions in the determination of ammonia was investigated. Received March 30, 2001 Revision September 3, 2001     

Elimination of the interferences of anions in the kinetic spectrophotometric determination of vanadium (V) solution

Accurate determination of vanadium (V) in industrial waste water is of great importance in environmental, biological and toxicological studies. Most of kinetic spectrophotometric methods based on the catalytic effect of vanadium (V), when applied to real samples for determination of trace levels of vanadium (V) lack the satisfactory sensitivity and selectivity. This may be attributed to the serious interferences of various anions which are common pollutants in industrial waste water. The oxidation of gallic acid by ammonium persulphate, catalysed by vanadium (V) was chosen for our study. The effect of the serious interferences of various anions such as chloride, bromate, bromide, chromate, iodide, iodate, molybdate, carbonate and sulphate on the net absorbance given by 4 microg l(-1) of vanadium (V) solution were studied. The minimum concentrations of citric acid, EDTA, ascorbic acid and oxalic acid as leveling off agents required to level off interfering effects due to the aforementioned anions in the kinetic determination of vanadium (V) were 50, 70, 80 and 120 microg ml(-1), respectively. In the presence of optimum concentrations of effective leveling off agents, the dynamic range can be extended and sensitivity increased as compared with the proposed method without levelling off agents. The proposed method is a rapid, sensitive and selective method for the determination of ultra trace amounts of vanadium (V) in real samples with satisfactory results.     

Fern constituents: triterpenoids from Adiantum capillus-veneris

Two new migrated hopane triterpenoids, viz. 4alpha-hydroxyfilican-3-one and fern-9(11)-en-12beta-ol, and olean-18-en-3-one and olean-12-en-3-one as the first example of oleanane compounds from Adiantum ferns were isolated along with many other known triterpenoids from Adiantum capillus-veneris of China and Egypt. Their structures were elucidated by spectroscopic analyses.     

Characterization of sintering of gelled UO3 microspheres

UO₃ microspheres, prepared using an internal gelation process, were reduced and sintered. Hydrogen and argon atmospheres were used at temperatures ranging from 1100 °C to 1400 °C for different durations.It was found that the sintered density is higher for spheres réduced at 700 °C than at any other reduction temperature. Lower densities were achieved in argon atmosphere than in hydrogen for the same sintering and reduction temperature. More than 98% Th.D. could be obtained by calcining the UO₃ spheres at 400 °C for 1 hr, reducing at 700 °C and then sintering at 1400 °C for 2 hrs in hydrogen atmosphere.

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Zusammenfassung Über interne Gebildungsprozesse hergestellte UO₃ Mikrokugeln wurden reduziert und gesintert. Dafür wurden Wasserstoff- und Argonatmösphären verschiedene Zeit lang bei Temperaturen zwischen 1100 °C und 1400 °C verwendet. Es wurde festgestellt, daß die Dichte des gesinterten Materials bei einer Reduktionstemperatur von 700 °C am größten ist. Bei gleichen Sinter- und Reduktionstemperaturen erreicht man in Argon eine geringere Dichte als in Wasserstoff. Mehr als 98% Th.D. kann man erreichen, indem man die UO₃ Kugeln bei 400 °C eine Stunde lang kalziniert, bei 700 °C reduziert und dann zwei Stunden lang bei 1400 °C in Wasserstoffatmosphäre sintert.

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, , . 1100–1400° . , , 700°, . . 98% 400° 1 , 700°, 2 1400°.

     

Effects of drying conditions on thermal decomposition behaviour of UO3 gel microspheres

The effects of the drying conditions on the thermal behaviour of UO₃ gel microspheres were studied by TG, DTA and X-ray examination. The effects of drying with air, steam or alcohol on the crystal structure and crystallite size were also studied. The results indicate that the thermal decomposition of UO₃ gel microspheres involves five steps: the first two for dehydration, the third for ammonia release, the fourth for ammonia oxidation, and the last one for UO₃ recrystallization. It was also found that the crystal growth varied from 110 Å after air drying to 512 Å and 496 Å after steam and alcohol treatment, respectively.

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Zusammenfassung Die Effekte der Trocknungsbedingungen auf das thermische Verhalten von UO₃-Gelmikrokugeln wurden mittels TG, DTA und Röntgenanalyse untersucht. Ebenfalls wurden die Auswirkungen der Trocknung mit Luft, Dampf und Alkohol auf die Kristallstruktur und die Kristallitgröße untersucht. Die Ergebnisse deuten darauf hin, daß die thermische Zersetzung der UO₃-Gelmikrokugeln in 5 Schritten verläuft: die ersten zwei sind Dehydratisierungsprozessen, der dritte der Freisetzung und der vierte der Oxydation von Ammoniak und der letzte der Rekristallisation des UO₃ zuzuschreiben. Die Kristallitgröße variiert zwischen 110 Å nach Lufttrocknung und 512 bzw. 496 Å nach Trocknung mit Dampf bzw. Alkohol.

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, UO₃ . , UO₃. , UO₃ : — , — , — — UO₃. , 110 Å 512 496 Å , , .

     

The mass spectra of nitrosulphanilamides. Observation of thermally generated products from 4-(piperidylsulphonyl)-2-nitroacetanilide

In addition to the expected electron impact induced fragmentation, the mass spectra of substituted nitrosulphanilamides, such as 4-(piperidylsulphonyl)-2-nitroacetanilide, exhibit peaks due to imidazoles, imidazole-N-oxides and furazans, which are formed thermally in the spectrometer ion source.     

Physico-Chemical Characteristics of Uranium Oxide Microspheres Produced by Internal Gelation

The developed Sol-Gel Hydrolysis Process was applied to produce uranium oxide microspheres suitable for use as nuclear fuel. Different preparation conditions of washing, feed solution aging and microsphere soaking were tried to produce dense UO₃- and UO₂-micospheres. The effect of reduction time and temperature on the density and porosity of the microspheres was carried out to optimize the preparation parameters. The total surface area, total pore volume and pore radius of UO₃- and UO₂-microspheres were measured through N₂ gas adsorption and application of the BET-equation at 77 K. The effect of the preparation conditions on crystallite size of the samples was made through ray diffraction analysis. Examination of the prepared uranium oxides by differential thermal analysis and thermal gravimetric analysis was carried out.     

Cosmogenic beryllium-7 in soil,rainwater and selected plant species to evaluate the vegetal interception of atmospheric fine particulate matter

Beryllium-7 is a radionuclide produced in the upper atmosphere by cosmic-ray spallation with ions of carbon, oxygen and nitrogen. It is one of radionuclides that can be used to trace the fine particulate matter of 2.5-µm diameter (PM_2.5) and smaller. In this work, ⁷Be was determined in leaves of 10 plant species collected from streets, parks and open land and in 5 consecutive rains over Alexandria, Egypt. ⁷Be levels were also measured in soil covered by each type of plant as well as in the nearest uncovered soil to be reference values to determine its intercepted amount and consequently PM_2.5. The lowest interception, 17.7?%, was by Ficus elastica L., while Ficus retusa L. intercepted about 45?%. Radiologically, the annual effective dose due to the usage of Thymelea hirsute plant leaves as a medicine and Nicotiana glauca Graham for smoking were 0.013 and 0.66 µSv, respectively. The observed levels in rainwater indicated that ⁷Be decreased consecutively from 3.1 Bq kg^–1 in the first rain to 0.71 Bq kg^–1 in the last one during the 2016/2017 rain season. The wet deposition of ⁷Be is less than 1?% of its total deposition on the ground.     

Thermal and X-ray analysis studies of UO3 gel microspheres

The thermal decomposition behaviour of UO₃ gel microspheres has been studied. Thermal analysis involved DTA, TG, DTG and X-ray examination. The effects of washing the UO₃ gel microspheres with hot water and with ammonia solution were investigated, as were the effects of soaking the microspheres in ammonia solution before or after washing on the crystallite size. The results indicate that the thermal decomposition of UO₃ gel microspheres includes five steps: the first two for dehydration, the third for ammonia removal, the fourth for ammonia oxidation and the last step for UO₃ recrystallization.

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Zusammenfassung Die thermische Zersetzung von UO₃-Gelmikrokugeln wurde mittels DTA, TG, DTG und Röntgendiffraktometrie untersucht. Die Auswirkungen des Waschens der UO₃-Gelmikrokugeln mit heißem Wasser und mit Ammoniaklösungen sowie der Einfluß des Wässerns der Mikrokugeln vor und nach dem Waschen mit Ammoniaklösungen auf die Kristallitgröße wurden untersucht. Die thermische Zersetzung der UO₃-Gelmikrokugeln verläuft in 5 Schritten: in den ersten beiden erfolgt die Dehydratisierung, im dritten die Abgabe und im vierten die Oxydation von Ammoniak und schließlich im letzten Schritt die Rekristallisation von UO₃.

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, , ₃. , . , ₃ , , — , — , ₃.