THE INTERACTION OF BORON TRIFLUORIDE WITH HYDRAZINE

1961 ◽  
Vol 39 (5) ◽  
pp. 986-994 ◽  
Author(s):  
W. G. Paterson ◽  
M. Onyszchuk

Boron trifluoride and anhydrous hydrazine react rapidly at 25° invacuo yielding a 1:1 complex compound, BF3•N2H4 (m.p. 87°), while at higher temperatures, or with diethyl ether as solvent, they form complex mixtures containing 52.2 to 63.5 mole percent BF3; but in tetrahydrofuran solution the 2:1 adduct, 2BF3•N2H4 (m.p. 260°) is formed. The X-ray powder diffraction pattern of BF3•N2H4 consists of 28 lines from which a unit cell with triclinic symmetry was calculated. The thermal decomposition of BF3•N2H4 is complex, yielding in part N2, NH3, NH4BF4, and BN. Hydrolysis of BF3•N2H4 yields a mixture of hydroxyfluoroborate ions. At −80°, BF3•N2H4 absorbs NH3 to form a diammoniate which liberates NH3 slowly at higher temperatures. Partial displacement of BF3 from BF3•N2H4 by HCl and partial absorption of HCl by BF3•N2H4 occur simultaneously at 110°.Infrared spectra of BF3•N2H4 and 2BF3•N2H4 have been measured in the range of 4000 to 650 cm−1 and frequency assignments have been made.

1967 ◽  
Vol 20 (3) ◽  
pp. 415 ◽  
Author(s):  
IJ Bear

The thermal decomposition process of zirconium sulphate tetrahydrate has been studied. Dehydration, which takes place via a crystalline monohydrate phase, is accompanied by the loss of small amounts of sulphuric acid apparently resulting from internal hydrolysis of the compound. This process gives a non-stoicheiometric zirconium sulphate which may exist in several modifications depending on the vapour pressure of the sulphuric acid around the sample during dehydration. The vapour pressure of the sulphuric acid is in turn controlled by such factors as the particle size of the tetrahydrate preparation, the size of sample, and the temperature and technique used during heating. Equilibration experiments have shown that a-Zr(SO4)2 is the stable anhydrous form. The X-ray powder diffraction patterns of a- and γ- Zr(SO4)2 have been indexed. Above 650� all forms of Zr(SO4)2 decompose to cubic ZrO2 which transforms to monoclinic ZrO2 at 800�.


TAPPI Journal ◽  
2011 ◽  
Vol 10 (1) ◽  
pp. 17-23
Author(s):  
KEVIN TAYLOR ◽  
RICH ADDERLY ◽  
GAVIN BAXTER

Over time, performance of tubular backpulse pressure filters in kraft mills deteriorates, even with regular acid washing. Unscheduled filter replacement due to filter plugging results in significant costs and may result in mill downtime. We identified acid-insoluble filter-plugging materials by scanning electron microscope/energy-dispersion X-ray spectroscopy (SEM/EDS) and X-ray diffraction (XRD) analysis in both polypropylene and Gore-Tex™ membrane filter socks. The major filter-plugging components were calcium sulfate (gypsum), calcium phosphate (hydroxylapatite), aluminosilicate clays, metal sulfides, and carbon. We carried out detailed sample analysis of both the standard acid-washing procedure and a modified procedure. Filter plugging by gypsum and metal sulfides appeared to occur because of the acid-washing procedure. Gypsum formation on the filter resulted from significant hydrolysis of sulfamic acid solution at temperatures greater than 130°F. Modification of the acid-washing procedure greatly reduced the amount of gypsum and addition of a surfactant to the acid reduced wash time and mobilized some of the carbon from the filter. With surfactant, acid washing was 95% complete after 40 min.


1984 ◽  
Vol 49 (4) ◽  
pp. 936-943 ◽  
Author(s):  
Bohumil Hájek ◽  
Pavel Karen ◽  
Vlastimil Brožek

For the investigation of the products of reaction of yttrium oxide with carbon mixed in various proportions, the chemical and X-ray diffraction methods of analysis were combined with the gas chromatographic analysis of the mixture of hydrocarbons and hydrogen formed on the sample decomposition with water. The carboreduction of Y2O3 was examined at relatively low temperatures, convenient for obtaining the reaction intermediates in higher yields. At 1 600 °C and pressures of 10-3 Pa the reduction of a mixture of Y2O3 with carbon in a stoichiometric ratio of 1 : 7 yields YC2 in equilibrium with 20% of Y2OC phase. At lower carbon contents (down to the Y2O3 : C ratio of 1 : 2) tha fraction of the Y2OC phase increases up to approximately 30%. In addition to Y2O3, the reaction mixture contains also Y2C, Y2OC and a phase giving propyne on hydrolysis. The presence of traces of C3 hydrocarbons and small amounts of methane in the product of hydrolysis of the carbide sample prepared by the carbothermal reduction of the oxide can be explained in terms of the occurrence of the Y15C19 phase, probably substituted in part by oxygen, and of the Y2OC phase. The results are compared with those obtained previously for the Sc2O3 + C system.


RSC Advances ◽  
2020 ◽  
Vol 10 (73) ◽  
pp. 44699-44711
Author(s):  
Md. Tuhinur R. Joy ◽  
Nikhil C. Bhoumik ◽  
Shishir Ghosh ◽  
Michael G. Richmond ◽  
Shariff E. Kabir
Keyword(s):  
X Ray ◽  

The cluster [Os3(CO)10(μ-OH)(μ-H)] was obtained in 75% from the hydrolysis of [Os3(CO)10(NCMe)2].


Polymers ◽  
2021 ◽  
Vol 13 (12) ◽  
pp. 1979
Author(s):  
Ho In Lee ◽  
Yun Heo ◽  
Seung-Woon Baek ◽  
Da-Seul Kim ◽  
Duck Hyun Song ◽  
...  

Poly(L-lactic acid) (PLLA) has been used as a biodegradable vascular scaffold (BVS) material due to high mechanical property, biodegradability, and biocompatibility. However, acidic byproducts from hydrolysis of PLLA reduce the pH after the surrounding implanted area and cause inflammatory responses. As a result, severe inflammation, thrombosis, and in-stent restenosis can occur after implantation by using BVS. Additionally, polymers such as PLLA could not find on X-ray computed tomography (CT) because of low radiopacity. To this end, here, we fabricated PLLA films as the surface of BVS and divided PLLA films into two coating layers. At the first layer, PLLA film was coated by 2,3,5-triiodobenzoic acid (TIBA) and magnesium hydroxide (MH) with poly(D,L-lactic acid) (PDLLA) for radiopaque and neutralization of acidic environment, respectively. The second layer of coated PLLA films is composed of polydopamine (PDA) and then cystamine (Cys) for the generation of nitric oxide (NO) release, which is needed for suppression of smooth muscle cells (SMCs) and proliferation of endothelial cells (ECs). The characterization of the film surface was conducted via various analyses. Through the surface modification of PLLA films, they have multifunctional abilities to overcome problems of BVS effectively such as X-ray penetrability, inflammation, thrombosis, and neointimal hyperplasia. These results suggest that the modification of biodegradable PLLA using TIBA, MH, PDA, and Cys will have important potential in implant applications.


Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 230
Author(s):  
Pengcheng Ma ◽  
Hongying Yang ◽  
Zuochun Luan ◽  
Qifei Sun ◽  
Auwalu Ali ◽  
...  

Bacteria–mineral contact and noncontact leaching models coexist in the bioleaching process. In the present paper, dialysis bags were used to study the bioleaching process by separating the bacteria from the mineral, and the reasons for chalcopyrite surface passivation were discussed. The results show that the copper leaching efficiency of the bacteria–mineral contact model was higher than that of the bacteria–mineral noncontact model. Scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier-transform infrared (FTIR) were used to discover that the leaching process led to the formation of a sulfur film to inhibit the diffusion of reactive ions. In addition, the deposited jarosite on chalcopyrite surface was crystallized by the hydrolysis of the excess Fe3+ ions. The depositions passivated the chalcopyrite leaching process. The crystallized jarosite in the bacteria EPS layer belonged to bacteria–mineral contact leaching system, while that in the sulfur films belonged to the bacteria–mineral noncontact system.


2020 ◽  
Vol 21 (3) ◽  
pp. 781
Author(s):  
Isabel Iglesias ◽  
José A. Huidobro ◽  
Belén F. Alfonso ◽  
Camino Trobajo ◽  
Aránzazu Espina ◽  
...  

The hydrothermal synthesis and both the chemical and structural characterization of a diamin iron phosphate are reported. A new synthetic route, by using n-butylammonium dihydrogen phosphate as a precursor, leads to the largest crystals described thus far for this compound. Its crystal structure is determined from single-crystal X-ray diffraction data. It crystallizes in the orthorhombic system (Pnma space group, a = 10.1116(2) Å, b = 6.3652(1) Å, c = 7.5691(1) Å, Z = 4) at room temperature and, below 220 K, changes towards the monoclinic system P21/n, space group. The in situ powder X-ray thermo-diffraction monitoring for the compound, between room temperature and 1100 K, is also included. Thermal analysis shows that the solid is stable up to ca. 440 K. The kinetic analysis of thermal decomposition (hydrogenated and deuterated forms) is performed by using the isoconversional methods of Vyazovkin and a modified version of Friedman. Similar values for the kinetic parameters are achieved by both methods and they are checked by comparing experimental and calculated conversion curves.


2013 ◽  
Vol 69 (11) ◽  
pp. 1225-1228 ◽  
Author(s):  
Sara Wyss ◽  
Irmgard A. Werner ◽  
W. Bernd Schweizer ◽  
Simon M. Ametamey ◽  
Selena Milicevic Sephton

Hydrolysis of the methyl ester (±)-threo-methyl phenidate afforded the free acid in 40% yield,viz.(±)-threo-ritalinic acid, C13H17NO2. Hydrolysis and subsequent crystallization were accomplished at pH values between 5 and 7 to yield colourless prisms which were analysed by X-ray crystallography. Crystals of (±)-threo-ritalinic acid belong to theP21/nspace group and form intermolecular hydrogen bonds. An antiperiplanar disposition of the H atoms of the (HOOC—)CH—CHpygroup (py is pyridine) was found in both the solid (diffraction analysis) and solution state (NMR analysis). It was also determined that (±)-threo-ritalinic acid conforms to the minimization of negativegauche+–gauche−interactions.


Author(s):  
Christian Schreinemachers ◽  
Olivier Bollen ◽  
Gregory Leinders ◽  
Václav Tyrpekl ◽  
Giuseppe Modolo ◽  
...  

2011 ◽  
Vol 89 (8) ◽  
pp. 971-977
Author(s):  
Danielle M. Chisholm ◽  
Robert McDonald ◽  
J. Scott McIndoe

Methylation of aromatic amino groups is usually straightforward, but the formation of two intramolecular hydrogen bonds in 3,3′-N,N′-bis(amino)-2,2′-bipyridine and (or) the potential for ring methylation prevents the clean tetramethylation of this molecule. Numerous attempts to make 3,3′-N,N′-bis(dimethylamino)-2,2′-bipyridine produced only complex mixtures of variously methylated products, and the only isolated molecule was 3,3′-N,N′-bis(methylamino)-2,2′-bipyridine, for which an X-ray crystal structure was obtained.


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