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György Dombi Éva Kalmár Gerda Szakonyi Henriett Diána Szűcs

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György Dombi Éva Kalmár Gerda Szakonyi Henriett Diána Szűcs University of Szeged Pharmaceutical Analysis Practicals Edited by: György Dombi Gerda Szakonyi Authors: György Dombi Éva Kalmár Gerda Szakonyi Henriett Diána Szűcs Reviewed by: Krisztina Novák-Takács Szeged, 2015 This work is supported by the European Union, co-financed by the European Social Fund, within the framework of "Coordinated, practice-oriented, student-friendly modernization of biomedical education in three Hungarian universities (Pécs, Debrecen, Szeged), with focus on the strengthening of international competitiveness" TÁMOP-4.1.1.C-13/1/KONV-2014-0001 project. The curriculum can not be sold in any form! TABLE OF CONTENTS CONDUCTOMETRY ....................................................................................................................... 3 CONDUCTOMETRIC TITRATION OF CARBOXYLIC ACIDS .............................................................. 7 ANALYSIS OF ACETYLSALICYLIC ACID ....................................................................................... 8 ANALYSIS OF BENZOIC ACID ........................................................................................................ 9 POTENTIOMETRIC (pH-METRIC) TITRATIONS ............................................................................ 10 HOW TO USE THE GLASS ELECTRODE ....................................................................................... 15 POTENTIOMETRIC TITRATION .................................................................................................... 15 EVALUATION OF THE MEASUREMENT ....................................................................................... 15 QUANTITATIVE ASSAYS BY TITRATION WITH ALKALINE SOLUTIONS ........................................ 16 DINATRII PHOSPHAS DIHYDRICUS ............................................................................................. 17 NATRII DIHYDROGENOPHOSPHAS DIHYDRICUS ......................................................................... 18 CHININI HYDROCHLORIDUM ..................................................................................................... 19 UNGUENTUM AD VULNERA ....................................................................................................... 21 SPECTROPHOTOMETRY .............................................................................................................. 23 PULVIS CHINACISALIS CUM VITAMINO C .................................................................................. 33 TABLETTA ASPIRINI 500 (ASPIRIN TABLET 500) ....................................................................... 37 SUPPOSITORIUM PARACETAMOLI 500 MG .................................................................................. 39 SPARSORIUM ANTISUDORICUM ................................................................................................. 41 SOLUTIO METRONIDAZOLI ........................................................................................................ 43 PULVIS CHOLAGOGUS ............................................................................................................... 44 DETERMINATION OF PROTEIN CONCENTRATION WITH THE BIURET REAGENT .......................... 47 ATOMIC ABSORPTION SPECTROMETRY ..................................................................................... 49 DETERMINATION OF MAGNESIUM CONTENT OF SPARSORIUM ANTISUDORICUM BY FLAME ATOMIC ABSORPTION ................................................................................................................ 53 DETERMINTION OF MAGNESIUM CONTENT OF PULVIS NEUTRACIDUS BY FLAME ATOMIC ABSORPTION ............................................................................................................................. 54 DETERMINATION OF ACTIVE INGREDIENTS OF PANADOL EXTRA BY HPLC .............................. 55 COMPLEXOMETRIC TITRATIONS ................................................................................................ 58 PULVIS NEUTRACIDUS ............................................................................................................... 63 SUSPENSIO ZINCI AQUOSA ........................................................................................................ 65 ARGENTOMETRIC ANALYSIS ..................................................................................................... 66 SPARSORIUM SULFABORICUM ................................................................................................... 67 REDOX TITRATIONS .................................................................................................................. 68 SUPPOSITORIUM ANTIPYRETICUM PRO INFATE VEL PRO PARVULO ........................................... 74 INJECTIO ALGOPYRINI 50% ....................................................................................................... 76 ACIDBASE TITRATIONS ........................................................................................................... 77 SPIRITUS IODOSALICYLATUS ..................................................................................................... 80 TEST YOURSELF – SAMPLE TEST QUESTIONS ............................................................................ 82 APPENDIX .............................................................................................................................. 92 UNICAM UV/VIS SPECTROPHOTOMETER MANUAL .................................................................. 93 UV-1601 SHIMADZU SPECTROPHOTOMETER MANUAL ............................................................. 95 MARS CEM MICROWAVE DESTRUCTOR MANUAL ..................................................................... 97 ATOMIC ABSORPTION SPECTROMETER MANUAL ...................................................................... 98 HPLC MANUAL ...................................................................................................................... 100 NMR SPECTRA ........................................................................................................................ 109 2 CONDUCTOMETRY (MEASUREMENT OF SPECIFIC CONDUCTANCE) Conductometry is based on the measurement of the conductance of electrolyte solutions. The passage of electric current through a chemical cell is carried out by the ionic species in the solution. It is an additive property, with the participation of all of the ions in the solution. The conductance is specified by the measurement of the resistance of a certain segment of the solution. The conductance (G) is the reciprocal of the resistance (R), its unit is 1/Ω Siemens; S): 1 G = R The conductance is directly proprotional to the surface area (A) of the electrodes and inversely proportional to the distance (d) between the electrodes: 1 A = κ R d κ is the specific conductance, where the resistance of the solution is measured between two electrodes of 1 cm2 area 1 cm apart. The conductance depends on the number of ions in the solution and on the identity of the ions. Some ions move faster than others in an electric field, and their mobility is therefore an important factor too. Dilution of an electrolyte solution will decrease the specific conductance: the lower number of ions present in a given volume, the lower the current flow is. The molar specific conductance () was introduced to characterize of the conductance of certain ions: = 1000 c where c is the concentration of the electrolyte solution. The ions in an infinitely dilute solution contribute to the conductance independently from each other, and the molar specific conductance of an infinite dilute solution can therefore be calculated by summing the conductances of each of the ions in the solution: and are the conductances of cations and anions, respectively in infinitely dilute solution. 3 The electrode Special eletrodes are used during conductometric measurements. The conductance is determined by measurement of the resistance of the solution in a certain volume between two electrodes made of platinized platinum. The surface area of the electrodes is increased and the polarization resistance is decreased by platinization. The electrodes are fixed tightly in a cylindrical unit. The fixed geometry specifies the distance of the electrodes during both the calibration and the measurement. Alternate current is used for the conductometric analysis so as to avoid disturbing electrode processes. A Wheatstone bridge is used to measure the resistance. Concentration measurement (direct conductometry) and conductometric titrations (indirect conductometry) are distinguished in conductometry. In direct conductometry, the concentration is determined by the measurement of conductance. This method is used, for example, to check Aqua purificata or Aqua destillata. An electrode is built into the ion-exchange system that continuously monitors the conductance of ion-exchanged water. When the conductance is above a given limit, the system must be regenerated. According to the European Pharmacopoeia 8th Edition, the maximum allowed conductance of Aqua purificata is 4.3 μS/cm, while that of Aqua ad iniectabilia is 1.1 μS/cm. Conductometric titrations can be applied when the ion concentration changes during a reaction, or when the ion concentration remains constant, but the mobility of the ions changes. Types of conductometric titrations Acid–base titrations It is easy to determine the equivalence point in these titrations because hydrogen ions (H+) are the most mobile of all ions, and hydroxide ions (OH-) are the second most mobile, and the mobilities are well above those of
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