The monothiocyanato-mercuric(II) nitrate [Hg(SCN)NO3] reagent has been prepared synthetically in
an aqueous medium and subjected for studies of titrimetric analysis of chloride concentration in beers.
In this studies, a measured volume of beer sample was added into known and an excess amount of
Hg(SCN)NO3 reagent and the surplus Hg(SCN)NO3 was determined by back titration against standard
potassium thiocyanate (KSCN) solution using ferric nitrate [Fe(NO3)3] indicator. The chloride ion and
Hg(SCN)NO3 were found to be reacting in the 1:1 stoichiometric ratio. The amount of chloride in beer
was determined with the amount of Hg(SCN)NO3 utilized in the titration reaction. The presence of
organic and inorganic materials had no effect on the titrimetric assay of chloride concentration in
beers as proved by the chloride recovery experiment. The statistical analysis of results showed average
standard deviation of 0.01034 and average relative error 1.12%, which indicates the accuracy of the
procedure.
A simple, rapid and improved visible spectrophotometric method has been proposed for determination of paracetamol (N-acetyl-p-aminophenol) in bulk drug. The experiment is based on the alkaline hydrolysis of paracetamol (PCT) to p-aminophenol (PAP) at elevated temperature and subsequent derivatization of PAP with sodium nitroprusside (SNP) at room temperature to produce an intense green colored N-nitrosyl-O-nitrosyl-p-aminophenol chromophore for direct determination of PCT at 685 nm. The molar absorptivity and Sandell's sensitivity are observed as 5.933x10 4 L.mol-1 .cm-1 and 0.0252 µg. cm-2 respectively for the chromophore. Beer's law is obeyed over the concentration range of 15-120 µg with linear regression equation as A= 0.009+0.003C (µg at 10 mL dilution). The percent recovery was found in the range 100.07-100.60%. The average of relative error and relative standard deviation are observed as 0.252% and 0.406% respectively. Reaction mechanism and reaction stoichiometry of the chromophoric reaction are discussed. The parameters with regard to determination of paracetamol by proposed method are optimized. Drugs like ibuprofen, aspirin and metformin do not interfere hence the proposed method is suitable for determination of PCT impurity in the said drugs.
The mono-thiocyanato mercuric (II) chloride [Hg(SCN)Cl] reagent was prepared synthetically and implemented for spectrophotometric determination of chloride in beers. In determining chloride, a known aliquot of beer sample was added into Hg(SCN)Cl reagent. The displaced thiocyanate ions were subsequently used to form the red-colored ferric-thiocyanate complex. The absorbance of which was measured at 455-nm was found directly proportional to the concentration of chloride in the beer sample. The experiment was performed by the standard addition method using beer sample and reagent at a time, and further various amount of known chloride was added during the measurement of absorbance. The analysis results show an average standard deviation of 0.02513. The output of this study provides evidence that, the Hg(SCN)2 reagent does not obey Beer’s law, whereas an excellent linearity of absorbance versus concentration of chloride was observed with the ratio of the concentration of Hg(SCN)Cl to chloride is less than 6.66.
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