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8 029 5003 - rfpc.ir

Practical TitrationTraining Manual for Titrimetric Volumetric AnalysisProf. Dr. Leo GrosEuropa Fachhochschule FreseniusLimburger Strasse 2DE-65510 Idstein/Taunus (Germany)Peter A. Bruttel and Marcus von KloedenMetrohm 68CH-9101 Herisau (Switzerland)The authors would like to express their thanks to Ms. Kathrin Sager, Metrohm Ltd., and Messrs. Volker Beenders and Kevin M ller, Europa Fachhochschule Fresenius, for carrying out the practical rights reserved, including those of by Metrohm Ltd., CH-9101 Herisau, 2005-052 Titrimetric analysis with Titrino or TitrandoPractical of Titration 32 Titrimetric analysis with Titrino or TitrandoPractical of Titration 3 PrefaceRecently a college lecturer was told that in the Geological Institute of a University the deter-minations of content were basically to be carried out by instrumental methods alone, for ex-ample atomic spectroscopy.

2 Titrimetric analysis with Titrino or Titrando Practical of Titration 3 Preface Recently a college lecturer was told that in the Geological Institute of a University the deter-

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1 Practical TitrationTraining Manual for Titrimetric Volumetric AnalysisProf. Dr. Leo GrosEuropa Fachhochschule FreseniusLimburger Strasse 2DE-65510 Idstein/Taunus (Germany)Peter A. Bruttel and Marcus von KloedenMetrohm 68CH-9101 Herisau (Switzerland)The authors would like to express their thanks to Ms. Kathrin Sager, Metrohm Ltd., and Messrs. Volker Beenders and Kevin M ller, Europa Fachhochschule Fresenius, for carrying out the practical rights reserved, including those of by Metrohm Ltd., CH-9101 Herisau, 2005-052 Titrimetric analysis with Titrino or TitrandoPractical of Titration 32 Titrimetric analysis with Titrino or TitrandoPractical of Titration 3 PrefaceRecently a college lecturer was told that in the Geological Institute of a University the deter-minations of content were basically to be carried out by instrumental methods alone, for ex-ample atomic spectroscopy.

2 The old-fashioned wet chemistry was no longer to be used. How good it is that students with experience in industrial laboratories can inform their teach-ers during their courses about all the applications in which the old-fashioned but still young titration method is being used in practice small book is based on the many years of experience gained by Metrohm in the devel-opment of instruments and applications. Peter Bruttel and Marcus von Kloeden have worked out the applications and collected them. The Europa Fachhochschule Fresenius (EFF) Id-stein, Germany, previously the Chemieschule Fresenius Wiesbaden, can look back on more than 150 years of practice-oriented teaching. Students of the EFF have tried out the practical examples. Since 1981 Leo Gros has taught analytical techniques at the EFF.

3 Marcus von Kloe-den was one of his students and became acquainted with Metrohm during a practical course abroad. The authors would like to thank Jan Volker Geil, Vice President, Metrohm Ltd., and himself a graduate of the EFF, for the many different ways in which he supported this project, as well as the EFF students Kevin M ller and Volker Beenders, who carried out the titrations . The authors would like to thank Heinz Gorbauch, their collegue of the Fresenius Institute and graduate of the EFF for his critical reading and additional Tutorial is primarily intended for training purposes but can also, of course, be used to advantage in any laboratory. It is intended to explain the theory in a simple manner and, by using practical examples, demonstrate just how versatile and accurate titrimetric analyses are.

4 The individual methods and procedures also provide the reader with many useful tips and explanations. This book is a practical manual not a detailed textbook and cannot and will not replace textbooks (see list of literature references in the Appendix)! Nevertheless, in order to be able to understand the practical applications better, some of the theory concern-ing types of reaction, substances and methods is briefly titrations can be carried out with any Metrohm titrator (Titrando, Titrino, Titroprocessor) as a matter of aspectsPlease note that this manual contains no information about the dangers related to the toxic-ity of the chemicals used nor about their disposal and handling. Please obtain the necessary knowledge from other sources. The chemicals used can be obtained from any qualified sup-plier.

5 Any mention of manufacturers in the practical part is just meant to indicate with which chemicals the experiments were carried hope that you will have a lot of pleasure and success with your work,Your Metrohm Ltd. and Europa Fachhochschule Fresenius (EFF)4 Titrimetric analysis with Titrino or TitrandoPractical of Titration 5 Table of contentsI. Theoretical part Titration Indication Titrants: preparation and titer Practical partII. 1 Acid-base titrations and methods, Electrode calibration and electrode Titer determination of hydrochloric acid, c(HCl) = mol/L with Titer determination of hydrochloric acid, c(HCl) = mol/L and validation of the 1 4 Titration of Titration of NaOH containing a small amount of Titration of sulfuric acid (H2SO4).

6 63II. Titration of acetic acid, DET and endpoint titration (SET)..65II. Titration of phosphoric acid (H3PO4), DET and Titration of boric acid (H3BO3) with and without addition of Titration of the acid and base capacity (p and m values) with fixed EPs and calculation of the carbonate Formol number in vegetable 2 Acid-base titrations and methods, non-aqueousII. General and additional remarks about non-aqueous Titer determination of perchloric acid, c(HClO4) = mol/L in glacial acetic Titer determination of alcoholic c(KOH) = Titration of nitrating acid (HNO3 / H2SO4 mixture)..84II. Acid number in petrochemical products with alcoholic Determining the ephedrine hydrochloride content according to Pharm. Determining the ephedrine hydrochloride content according to USP 24 Benzoic acid in H2O, ethanol, acetone, MIBK and Aniline in H2O, ethanol, acetone, dioxan/IPA and 3 Precipitation Titer determination of c(AgNO3) = Chloride (NaCl) in meat Chloride in drinking Sulfide in Cyanide in Mixture of chloride, bromide and iodide with and without added Cationic surfactant in mouth Anionic surfactants and soaps in washing powder, potentiometric two-phase Calibration factor for nonionic Nonionic surfactants in household Titrimetric analysis with Titrino or TitrandoPractical of Titration 5II.

7 4 Redox titrations and methodsII. Iodometry (iodine/thiosulfate)..115II. Thiosulfate with iodine, potentiometric, biamperometric and bivoltametric Bromine index in petrochemical Free sulfurous acid (SO2) in Oxygen content in water, Winkler Hydrogen peroxide (H2O2) in disinfectants, with Diazotization titration with 5 Complexometric and chelometric methodsII. Titer determination of c(Na2 EDTA) = mol/L with Ca and sulfate content in tap water with the Ca Ca and Mg content (total hardness) in water with the Ca Total hardness in drinking water with the Ca Total hardness in drinking water with the Spectrosense 610 Nickel in a nickel electroplating bath with the Cu Calcium in milk with the Cu Aluminum in antacids with the Spectrosense 610 Iron in cement with the Spectrosense 610 Appendix Further and/or cited literature standardized 275 years the history of titrimetric Titrimetric analysis with Titrino or TitrandoPractical of Titration 76 Titrimetric analysis with Titrino or TitrandoPractical of Titration 7I.

8 1 Introduction: titration means counting!Together with gravimetry, titration is one of the oldest analytical methods. Both belong to a group of analytical methods that is based on chemical a titration one determines the volume of a standard solution (titrant) that is necessary for complete chemical reaction with the analyte. The titrant contains a known amount of a par-ticular Loschmidt and Avogadro we know that one gram molecule of a substance contains a defined number of particles. A standard solution is produced by dissolving a particular weight of a substance in a solvent. Each volume fraction of this standard solution contains a defined number of particles of the dissolved substance. This means that measuring the volume of a standard solution is a method of counting particles: Titration means counting!

9 Despite many new, mainly physical instrumental analytical methods, titrimetry as a wet-chemistry method still remains a standard procedure for quantitative analysis today. This is because it has a number of specific advantages: Titration is one of the absolute content determination methods, the result of the analy-sis provides direct information about the amount of substance to be determined, without instrument or method-specific factors having to be calibrated (such as is normal in relative methods, for example HPLC, atomic spectroscopy or UV/VIS photometry). titrations are easy to carry out: The equipment and the procedures to be performed are simple. They are easy to understand the fundamentals of titrimetric methods are widely known or can be learned in a short time.

10 titrations are carried out rapidly: If the total time for setting up the workplace to obtain-ing the analytical result is taken into consideration, then titrimetric determinations require much less time than other methods. Titration is a versatile method: Numerous titration methods have been drawn up, these range from the determination of inorganic ions up to the determination of complex organic compounds. The analyte concentrations can range from 100% or virtually 100% (analysis of ultrapure substances, purity determinations) down to the ppm range. Sample amounts of a few micrograms are adequate, amounts in the gram range are also possible. Titration supplies highly reproducible and correct results. A typical reproducibility is <1%. In high-precision titrations values of are demanded and also achieved.


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