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.
Objective: A selective mercurimetric titration procedure is proposed for the assay of chloride concentration in the water of green coconut using mercury (II) nitrate [(Hg(NO3) Methods: An indicator solution was prepared by titrating Hg(NO3)2 against potassium thiocyanate (KSCN) till a red color end point using Fe(NO3)3. Then a known amount of Hg(NO3)2 was added to indicator solution and titrated against the water of green coconut till the original red color reappeared. Results:The concentration of chloride present in the volume of coconut water utilized in between these two end points was found to be reacting in the 2:1 stoichiometric ratio with the Hg(NO3)2 taken in the second step of the titration. The statistical treatment of the experimental data obtained by using standard solutions of sodium chloride (NaCl) indicates that the procedure is precise and accurate. The phosphate, sulfate, organic compounds and inorganic minerals present in the coconut water did not interfere with the measurement of chloride by this procedure. Both the cationic mineral value (was also determined by complexometric titration) and chloride concentration in the coconut water were found to be decreased with the development of the coconuts. Conclusion:The proposed procedure of determination of chloride concentration in the water of green coconut is simple, reliable and inexpensive. This procedure is excellent for determination of chloride in the acidic solution without precise adjustment of the pH for detection of the end point. Owing to the homogenous reaction condition no titration errors those are commonly encountered by co-precipitation in the argentometric assay of chloride.
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.
A simple, rapid, reliable and novel titration procedure for the mercurimetric assay of metformin hydrochloride (MHCl) based on measurement of the chloride content of its hydrochloride salt is described. In this experiment, initially a synthetic mercury(II) thiocyanate [Hg(SCN)2] indicator was prepared by titrating mercury(II) nitrate [Hg(NO3)2] against potassium thiocyanate (KSCN) in the 1:2 stoichiometric ratio using ferric nitrate [Fe(NO3)3]. After addition of a known amount of Hg(NO3)2 to the indicator, the solution was further titrated against the aqueous solution of MHCl until the original red color reappeared. The concentration of chloride present in the volume (of MHCl) utilized for the reaction was found to be reacting in the 2:1 stoichiometric ratio with the Hg(NO3)2 taken in the second titration. The statistical treatment of the experimental data obtained by determining MHCl in the concentration range 0.8281 to 8.281 g/lit, indicates that the procedure is precise and accurate. The procedure was further applied for the analysis of MHCl in tablet formulations. The average recovery and accuracy were found to be in agreement with claimed by the manufacturer. The common excipients used in tablet formulations did not interfere in the determination of MHCl by this procedure as observed by the recovery experiment using standard addition method. The chemistry involved in titration, the action of an indicator at the end point and the factors that affecting the reaction stoichiometry are discussed. Keywords: Chloride assay, Mercurimetric titration, Mercury (II) nitrate, Mercury(II) thiocyanate-iron(III) nitrate indicator system, Metformin hydrochloride, Metformin hydrochloride tablets.
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