Test Method for Formic Acid in Glacial Acetic Acid

10.1520/d3546 ◽  
2008 ◽  
Author(s):  
1957 ◽  
Vol 35 (12) ◽  
pp. 1417-1422 ◽  
Author(s):  
C. C. Lee ◽  
G. P. Slater ◽  
J. W. T. Spinks

The solvolysis of 2-phenylethyl-1-C14p-toluenesulphonate in absolute ethanol, glacial acetic acid, 90% formic acid, and anhydrous formic acid gave rise to products which showed rearrangements of the C14-labeled atoms from the C-1 to the C-2 positions to the extent of 0.3%, 5.5%, 40%, and 45%, respectively. The results constitute an unequivocal proof that phenyl participation occurs in the reactions studied. The different degrees of rearrangement found for the different solvent systems are in agreement with the concept that the solvolysis process may have a range of mechanisms between the two extremes of the nucleophilic or SN2 type and the limiting or SN1 type. In the solvolysis in absolute ethanol, a small amount of "unreacted" 2-phenylethyl p-toluenesulphonate recovered from the reaction mixture was found to show isotope position rearrangement of almost the same degree as the ethanolysis product. This finding is tentatively attributed to the phenomenon of internal return involving an ethyl-phenonium p-toluenesulphonate ion-pair.


2011 ◽  
Vol 2011 ◽  
pp. 1-10 ◽  
Author(s):  
A. Gholipour Kanani ◽  
S. Hajir Bahrami

Polycaprolactone nanofibers were prepared using five different solvents (glacial acetic acid, 90% acetic acid, methylene chloride/DMF 4/1, glacial formic acid, and formic acid/acetone 4/1) by electrospinning process. The effect of solution concentrations (5%, 10%, 15% and 20%) and applied voltages during spinning (10 KV to 20 KV) on the nanofibers formation, morphology, and structure were investigated. SEM micrographs showed successful production of PCL nanofibers with different solvents. With increasing the polymer concentration, the average diameter of nanofibers increases. In glacial acetic acid solvent, above 15% concentration bimodal web without beads was obtained. In MC/DMF beads was observed only at 5% solution concentration. However, in glacial formic acid a uniform web without beads were obtained above 10% and the nanofibers were brittle. In formic acid/acetone solution the PCL web formed showed lots of beads along with fine fibers. Increasing applied voltage resulted in fibers with larger diameter.


1967 ◽  
Vol 50 (2) ◽  
pp. 354-360 ◽  
Author(s):  
Leonard Stoloff

Abstract A modification of the Andrellos procedure for identification of afiatoxin B1 was studied collaboratively in 19 laboratories. The procedure, based on the altered chromatographic behavior of the afiatoxin after reactions with trifluoroacetic acid, formic acid/thionyl chloride, and glacial acetic acid/thionyl chloride, was modified by an improved silica gel column cleanup and a clearer definition of sources of difficulty. Each collaborator examined 3 extract samples: two naturally contaminated with 5 μg afiatoxin B1/sample, and one aflatoxin-free extract to which an afiatoxin B2 artifact was added. No false identifications were made. Sixteen laboratories obtained reasonably good results with the trifluoroacetic acid and formic acid/thionyl chloride reagents. Twelve laboratories obtained reasonably good results with the acetic acid/thionyl chloride reagent but there was general difficulty with a side reaction assumed to be caused by inability to maintain anhydrous conditions. The method was recommended for adoption as official, first action.


2008 ◽  
Vol 59 (1) ◽  
pp. 41-44
Author(s):  
Maria-Daniela Sofei ◽  
Maria Ilici ◽  
Valentin Badea ◽  
Carol Csunderlik ◽  
Vasile-Nicolae Bercean

The synthesis of 1H-3-aryl-7-ethoxycarbonyl-6-methyl-pyrazolo[5,1-c][1,2,4]triazoles (2) was carried out by cyclization of 1H-5-arylidenehydrazino-4-ethoxycarbonyl-3-methyl-pyrazoles (1) in the presence of bromine using glacial acetic acid as solvent and sodium acetate as base. The new nine obtained compounds were characterized by IR and NMR spectroscopy and mass spectrometry.


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