The direct potentiometric titration of three antiinflammatory agents, namely mefenamic acid, fenbufen and ibuprofen. It showed satisfactory data for all the parameters of validation. The nonaqueous titration of bronsted acids and bases, a subject which has become. The procedure is based on the use of volumetric dosage in a nonaque ous medium in glacial acetic acid with 0. Vorlander first proposed the nonaqueous titration method that is titration of aniline with the hcl in nonaqueous solvent, that is, benzene. Pdf nonaqueous titrations is the most titrimetric procedure used in. Unknown 6 december at fritz first used this method to distinguish the aromatic and aliphatic amines by using the perchloric acid as titrant. Non aqueous titration is suitable for the titration of very weak acids and very weak bases. Nonaqueous phase titration acid number is defined as the quantity of base, expressed as milligrams of potassium hydroxide per gram of sample, required to titrate a sample to specified end point. The quantitation method of silc active pharmaceutical ingredient by non aqueous acidbase titration was developed using methanol as solvent and 0. The steps involved in the nonaqueous titrimetric method are proposed by the tomicek. The values of percentage recovery and standard deviation showed sensitivity. Determination of olanzapine by uv spectrophotometry and.
The method based on nonaqueous titration using acetous perchloric acid as a titrant and acetous crystal violet as indicator. Non aqueous titration definition, theory, and types of. Method a i for halide salts of organic bases dissolve a quantity of the substance being examined to give an expected titration volume of between 7090% of the burette volume, in 50 ml of dehydrated ethanol r and 5. According to this theory an acid is a proton donor and base is a proton acceptor. The water content of injections is removed by evaporation to a small bulk, and the last traces are allowed to react with a sufficient amount of acetic anhydride. Fritz first used this method to distinguish the aromatic and aliphatic amines by. A titration for acidity or basicity, rather than a ph measurement, may be appropriate for nonaqueous samples. Pdf nonaqueous titrimetric assay of gabapentin in capsules.
Titration of pharmaceuticals in nonaqueous solvents wiley online. Titration of bases the nonaqueous titration of weak bases with perchloric acid is the part of nonaqueous titrimetry that has been until now, most thoroughly dealt with. Nonaqueous titrations pharmaceutical analysis book. Vorlander first proposed the non aqueous titration method that is titration of aniline with the hcl in non aqueous solvent, that is, benzene. Nonaqueous titration of gatifloxacin in pharmaceutical.
Accordingly a simple and accurate procedure for their determination, based on their titration in acetic anhydrideacetic acid solvent system 5. There are alternate buffers available, such as water methanol and waterethanol buffer systems as described by iupac6. The method of determination by titration in nonaqueous media of bases and acids which are too weak to be titrated in aqueous solution has been investigated. Using this standardized solution, you will determine the acid neutralizing power of a commercially available antacid tablet. Consultation documents pdf, 253kb world health organization. A simple, costeffective, rapid, and precise method for determination of loratadine lor in pure and pharmaceutical dosage forms was developed. A substance can be weakly acidic and so it does not permit for precise analysis by direct titration.
The method based on nonaqueous titration using acetous perchloric. Non aqueous titration refers to a type of titration in which the analyte substance is dissolved in a solvent which does not contain water. A potentiometric titration method in nonaqueous media is proposed for the determination of some commonly used antiinflammatory agents. The proposed method of nonaqueous potentiometric titration was found to be precise, accurate and rugged.
Two new methods for the determination of olanzapine, based on uv spectrophotometry and nonaqueous titration, have been developed. In this experiment, you will standardize a solution of base using the analytical technique known as titration. The titration was carried out using standardized 0. Many reactions which have a small heat of reaction may thus cause a sufficient temperature change in a nonaqueous system to enable acceptable enthalpograms to be obtained, and. These are the titration done for organic and medicinal compounds. Development and validation of alternative methods by non. The first part considers the general principles of. Fia titrations of phenothiazine derivatives in aqueous. Development and validation of alternative methods by nonaqueous. The uv absorbance of the methanolic solution of olanzapine was. It is the most common titrimetric procedure used in pharmacopoeial. Such titration can also be used for the titration of those substance which are not soluble in aqueous solvent. The need for non aqueous titration arises because water can behave as a weak base and a weak acid as well, and can hence compete in proton acceptance or proton. It is suitable for assay of fdh in bulk drug and can be used as an analytical method to determine assigned values without the need fdh primary standard.
Non aqueous titrations, basic concepts, bronsted lowry concept, lweis concept, why non aqueous titration is used. The fia titration method in nonaqueous media based on an official method of determination titration with perchloric acid in anhydrous acetic acid was also developed. The nonaqueous titrimetric assay of the selected anti. The steps involved in the non aqueous titrimetric method are proposed by the tomicek. This procedure is a very important one in pharmacopoeial assays. Lowitz first prepared the moisturefree solvents non aqueous solvents.
A validated nonaqueous potentiometric titration method. Here, spiking method 1 is used, because astm american society for testing and materials standard procedure 2 requires. Nonaqueous titration of bases with perchloric acid. Visual indicator are formed to the most suitable for the detection of end point in nonaqueous titration. Non aqueous titration definition, theory, and types of non. The method permits a rapid determination of different types of compounds common in the. This application note describes a simple method for the determination of nicotine in tobacco using nonaqueous titration. Nonaqueous titrimetric determination of sulphadimidine sodium. Analysis outlining the method for nonaqueous titration of different bases with perchloric acid in glacial acetic acid using the schott instruments titroline 7750 multiparameter titrator, which conveniently combines the features of the potentiometric titrator and the volumetric karl fischer titrator. Introduction although ph measurements are primarily done on aqueous waterbased samples, there are many ph applications that call for ph measurements and titrations in nonaqueous samples or in mixed aqueousnonaqueous samples. Nonaqueous titration is the titration of substances dissolved in nonaqueous solvents. These are extremely weak and cannot be analysed using normal titrimetric methods.
These assays sometimes take some perfecting in terms. The organic acids and bases are insoluble in water. Under optimized reaction conditions and flowthrough parameters, the calibration range and equations, the sensitivity, and the repeatability of all methods were found and discussed. The most commonly used procedure is the titration of organic bases with perchloric acid in anhydrous acetic acid. Determination of nicotine in tobacco by nonaqueous titration. Lowitz first prepared the moisturefree solvents nonaqueous solvents.
Nonaqueous titration is the titration of substances dissolved in solvents other than water. The procedure of non aqueous titration is very useful because it satisfies two different requirements, namely suitable titration of very weak. Further, depending upon which part of a compound is physiologically active, it is often possible to titrate that part by proper selection of solvent and titrant. Used in the determination of the chloropheneramine. The main principle involved in the nonaqueous titrimetric method is the samples are dissolved in the nonaqueous solvents. Indicators for nonaqueous titrations the ionized and unionized or the different resonant forms of indicators are apply equally well for nonaqueous titrations but their colour changes at the end point vary from titration to titrations, as they depend on the nature of the titrant. These sample types can be challenging, but when you. Non aqueous titrations pdf different types of nonaqueous titrations and complete bibliographies on. Kf reagentskarl fischer discovered that the reaction performed in a nonaqueous system, i.
Acidbase titrations in nonaqueous solvents acs publications. Vorlander 85, using indicators, observed color changes with gaseous. In general, the concept of ph becomes a relative measurement in these samples. This is a method extrapolated to use titration for non readily reactive substances. The quantitation method of silc active pharmaceutical ingredient by nonaqueous acidbase titration was developed using methanol as solvent and 0. As a first step in phasing out mercurybased methods, it is proposed to revise chapter 2. Non aqueous titration are those titration in which titration of weak acidic or basic substance carried out using non aqueous substance.
Analysis in nonaqueous solvents is by no means a new technique. The results of the titration of chlorpromazine hydrochloride, according to the proposed visual nonaqueous titration method, are shown in table i. Nonaqueous titrations is the most titrimetric procedure used in pharmacopoeial assays and serves a double purpose, as it suitable for the titration of weak acids and bases and provides a solvent. A simple precise, rapid accurate and sensitive nonaqueous potentiometric titration method was developed for quantitative determination of azelnidipine from pharmaceutical dosage form. The important indicator used for nonaqueous titration are follow.
The proposed method was found to be precise with % rsd 7. Non aqueous phase titration acid number is defined as the quantity of base, expressed as milligrams of potassium hydroxide per gram of sample, required to titrate a sample to specified end point. Titrations in nonaqueous solvents discuss the theory, practice, and data on acidic and basic strength of nonaqueous solvents. This increase in the temperature change is reflected in the increased sensitivity of the method when used in a nonaqueous system. It is the most common titrimetric procedure used in pharmacopoeial assays and serves a double purpose. Nonaqueous titration of bases with perchloric acid titration. The non aqueous titration can be explained by the useing bronstedlowry theory. The application of titration in nonaaqueous media to. Pdf nonaqueous titrimetric assay for determination of. Titration of pharmaceuticals in nonaqueous solvents. Chemistry of nonaqueous titration of chlorpromazine pdf.
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