Nonaqueous Titration of Halides of Nitrogenous Bases, Using Trifluoromethyl Sulfonic Acid

1986 ◽  
Vol 69 (4) ◽  
pp. 620-624 ◽  
Author(s):  
N Aziz Zakhari ◽  
K Artur Kovar
Keyword(s):  
Acetic Acid ◽  
Acetic Anhydride ◽  
Perchloric Acid ◽  
Sulfonic Acid ◽  
Glacial Acetic Acid ◽  
Visual Detection ◽  
Phenothiazine Derivatives ◽  
Solvent Systems ◽  
Anhydrous Acetic Acid

Abstract Trifluoromethyl sulfonic acid in glacial acetic acid has been compared with perchloric acid as a titrant in 4 solvent systems: glacial acetic acid, acetic anhydride, a mixture of both, and acetone. The comparison was limited to the determination of halides of nitrogenous bases with and without the use of mercury(II) acetate reagent. The results of the visual titrations showed that both acids are comparable tit rants. However, trifluoromethyl sulfonic acid proved to be superior to perchloric acid in potentiometric titrations carried out in acetic acid-acetic anhydride mixtures. Moreover, the nonoxidizing properties exhibited by trifluoromethyl sulfonic acid proved advantageous over perchloric acid in the visual detection of end points in the titration of phenothiazine derivatives in anhydrous acetic acid, using crystal violet indicator.

Collaborative Study of Nonaqueous Titration Method for Dodine in Formulations

1969 ◽  
Vol 52 (6) ◽  
pp. 1292-1294
Author(s):  
N Robert Pasarela
Keyword(s):  
Acetic Acid ◽  
Acetic Anhydride ◽  
Perchloric Acid ◽  
Collaborative Study ◽  
Titration Method ◽  
Powder Formulation ◽  
Coefficients Of Variation ◽  
Wettable Powder ◽  
Metanil Yellow

Abstract A nonaqueous titration method for the determination of dodine in 65% wettable powder formulations was studied by ten collaborators. The dodine is extracted from the formulation with acetic acid-acetic anhydride (10 + 90). The extract is filtered, and the resultant acetylated compound in solution is basic enough to be titratable with perchloric acid at a relatively low potential. The titration is carried out potentiometrically or visually, using metanil yellow as an indicator. The coefficients of variation for re-dodecylguanidine acetate standard and the 65% wettable powder formulation were 0.24 and 0.55%, respectively. The method is recommended for adoption as official first action.

Determination of Piperazine in Formulations by Nonaqueous Titration

1963 ◽  
Vol 46 (6) ◽  
pp. 1060-1062
Author(s):  
R B Maybury ◽  
R Payfer
Keyword(s):  
Aqueous Solution ◽  
Acetic Acid ◽  
Perchloric Acid ◽  
Glacial Acetic Acid ◽  
Chloroform Solution ◽  
New Method ◽  
Alternative Procedure ◽  
Good Agreement

Abstract A new method is presented for the nonaqueous titration of piperazine in formulations in which the piperazine base is first brought into aqueous solution, and the solution is made strongly alkaline and extracted with chloroform. The chloroform solution of piperazine is then titrated with acetous perchloric acid to alpha-naphthol benzein indicator. The procedure is rapid, shows good agreement with other methods, and is applicable to most kinds of piperazine formulations. An alternative procedure for piperazine adipate, citrate, or tartrate in powders is given, in which the compound is dissolved and titrated directly in glacial acetic acid.

scholarly journals Oxidation of 3-Carene with Red Lead in Glacial Acetic Acid and Acetic Anhydride

1974 ◽  
Vol 23 (7) ◽  
pp. 420-422
Author(s):  
Yoshiharu MATSUBARA ◽  
Yoshihito FUJIHARA ◽  
Yutaka SAKAI ◽  
Makoto SANO
Keyword(s):  
Acetic Acid ◽  
Acetic Anhydride ◽  
Glacial Acetic Acid ◽  
Red Lead

Reverse Phase Liquid Chromatographic Determination of Chlorophacinone and Diphacinone in Bait Formulations

1982 ◽  
Vol 65 (4) ◽  
pp. 927-929
Author(s):  
Brian R Bennett ◽  
Gregory S Grimes
Keyword(s):  
Acetic Acid ◽  
Glacial Acetic Acid ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Target Concentration ◽  
External Standard ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract Chlorophacinone and diphacinone are extracted at the 0.005% level from grain or paraffinized baits with glacial acetic acid. The target concentration is 0.01 mg/mL. The filtered supernate is chromatographed on a Partisil PXS ODS10/25 liquid chromatography column with premixed and degassed glacial acetic acid-tetrahydrofuran-water (14 + 2 + 9) and detected at 288 nm. The concentration is calculated by using an external standard. The recovery from spiked samples averaged 96.6% for both analytes. The response is linear from 0.001 to 0.040 mg/mL. The coefficient of variation of within-day replicates ranged from 1.1 to 2.5%.

1,4-Dinitroimidazole and Derivatives. Structure and Thermal Rearrangement

1989 ◽  
Vol 42 (8) ◽  
pp. 1281 ◽  
Author(s):  
MR Grimmett ◽  
ST Hua ◽  
KC Chang ◽  
SA Foley ◽  
J Simpson
Keyword(s):  
Molecular Structure ◽  
Acetic Acid ◽  
Acetic Anhydride ◽  
Glacial Acetic Acid ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Thermal Rearrangement

Nitration of 4-nitroimidazole in acetic anhydride/glacial acetic acid gives 1,4-dinitroimidazole. The crystal and molecular structure of this compound have been determined by direct methods. Crystals are orthorhombic; P212121, a 5.853(3), b 9.591(8), c 10.392(5) � , V 583.4(7) � 3 , Dm 1 .76 g cm-1, Dc, 1 .80 g cm-1 (Z = 4); λ 0.71069 � ; T 173 K. The structure was refined to R = 0.048 for 926 reflections [I > 2 σ(1)]. Both 2-methyl-4-nitro- and 5-methyl-4-nitro-imidazoles N-nitrate under the same conditions. When heated in solution at 100-140�C 1,4-dinitro- and 2-methyl-1,4-dinitro-imidazoles rearrange to give C-nitro isomers and some denitration products, but 5(4)-methyl-1,4(5)-dinitroimidazole failed to give identifiable products.

Method for the accurate determination of specific rotation. Specific rotation of valine and leucine

1969 ◽  
Vol 47 (15) ◽  
pp. 2739-2746 ◽  
Author(s):  
J. C. MacDonald
Keyword(s):  
Acetic Acid ◽  
Glacial Acetic Acid ◽  
Optical Rotation ◽  
Accurate Determination ◽  
Computer Calculation ◽  
Specific Rotation ◽  
Best Fit

The optical rotation of various concentrations of L-valine and L-leucine, dissolved in glacial acetic acid, or 5 or 6 M HCl, was measured with a photoelectric polarimeter at the nominal wavelengths 589, 578, 546, 436, and 365 nm and temperatures of 20, 25, and 30 °C. The specific rotation for any one wavelength, solute, and solvent could be defined by the equation [α]λT = A(1 + D(T − 25)) + BC, where T is temperature in °C, C is concentration in grams of solute per 100 ml of solution, and A, B, and D are constants. The best fit values of the constants were determined by computer calculation and are listed. Constants are also given for calculating a specific rotation based on grams of solute per 100 g of solution.

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