An Introductory Course of Quantitative Chemical Analysis | Page 2

has been changed to introduce volumetric procedures first. Teachers who are familiar with earlier editions will, however, find that the order of presentation of the material under the various divisions is nearly the same as that previously followed, and those who may still prefer to begin the course of instruction with gravimetric processes will, it is believed, be able to follow that order without difficulty.
Procedures for the determination of sulphur in insoluble sulphates, for the determination of copper in copper ores by iodometric methods, for the determination of iron by permanganate in hydrochloric acid solutions, and for the standardization of potassium permanganate solutions using sodium oxalate as a standard, and of thiosulphate solutions using copper as a standard, have been added. The determination of silica in silicates decomposable by acids, as a separate procedure, has been omitted.
The explanatory notes have been rearranged to bring them into closer association with the procedures to which they relate. The number of problems has been considerably increased.
The author wishes to renew his expressions of appreciation of the kindly reception accorded the earlier editions of this manual. He has received helpful suggestions from so many of his colleagues within the Institute, and friends elsewhere, that his sense of obligation must be expressed to them collectively. He is under special obligations to Professor L.F. Hamilton for assistance in the preparation of the present edition.
HENRY P. TALBOT
!Massachusetts Institute of Technology, September, 1921!.

CONTENTS


PART I. INTRODUCTION
SUBDIVISIONS OF ANALYTICAL CHEMISTRY
GENERAL DIRECTIONS Accuracy and Economy of Time; Notebooks; Reagents; Wash-bottles; Transfer of Liquids


PART II. VOLUMETRIC ANALYSIS
GENERAL DISCUSSION Subdivisions; The Analytical Balance; Weights; Burettes; Calibration of Measuring Devices GENERAL DIRECTIONS Standard and Normal Solutions
!I. Neutralization Methods!
ALKALIMETRY AND ACIDIMETRY Preparation and Standardization of Solutions; Indicators STANDARDIZATION OF HYDROCHLORIC ACID DETERMINATION OF TOTAL ALKALINE STRENGTH OF SODA ASH DETERMINATION OF ACID STRENGTH OF OXALIC ACID
!II. Oxidation Processes!
GENERAL DISCUSSION BICHROMATE PROCESS FOR THE DETERMINATION OF IRON DETERMINATION OF IRON IN LIMONITE BY THE BICHROMATE PROCESS DETERMINATION OF CHROMIUM IN CHROME IRON ORE PERMANGANATE PROCESS FOR THE DETERMINATION OF IRON DETERMINATION OF IRON IN LIMONITE BY THE PERMANGANATE PROCESS DETERMINATION OF IRON IN LIMONITE BY THE ZIMMERMANN-REINHARDT PROCESS DETERMINATION OF THE OXIDIZING POWER OF PYROLUSITE IODIMETRY DETERMINATION OF COPPER IN ORES DETERMINATION OF ANTIMONY IN STIBNITE CHLORIMETRY DETERMINATION OF AVAILABLE CHLORINE IN BLEACHING POWDER
!III. Precipitation Methods!
DETERMINATION OF SILVER BY THE THIOCYANATE PROCESS


PART III. GRAVIMETRIC ANALYSIS
GENERAL DIRECTIONS Precipitation; Funnels and Filters; Filtration and Washing of Precipitates; Desiccators; Crucibles and their Preparation for Use; Ignition of Precipitates DETERMINATION OF CHLORINE IN SODIUM CHLORIDE DETERMINATION OF IRON AND OF SULPHUR IN FERROUS AMMONIUM SULPHATE DETERMINATION OF SULPHUR IN BARIUM SULPHATE DETERMINATION OF PHOSPHORIC ANHYDRIDE IN APATITE ANALYSIS OF LIMESTONE Determination of Moisture; Insoluble Matter and Silica; Ferric Oxide and Alumina; Calcium; Magnesium; Carbon Dioxide ANALYSIS OF BRASS Electrolytic Separations; Determination of Lead, Copper, Iron and Zinc. DETERMINATION OF SILICA IN SILICATES


PART IV. STOICHIOMETRY
SOLUTIONS OF TYPICAL PROBLEMS PROBLEMS
APPENDIX
ELECTROLYTIC DISSOCIATION THEORY FOLDING OF A FILTER PAPER SAMPLE NOTEBOOK PAGES STRENGTH OF REAGENTS DENSITIES AND VOLUMES OF WATER CORRECTIONS FOR CHANGE OF TEMPERATURE OF STANDARD SOLUTIONS ATOMIC WEIGHTS LOGARITHM TABLES

QUANTITATIVE CHEMICAL ANALYSIS


PART I
INTRODUCTION
SUBDIVISIONS OF ANALYTICAL CHEMISTRY
A complete chemical analysis of a body of unknown composition involves the recognition of its component parts by the methods of !qualitative analysis!, and the determination of the proportions in which these components are present by the processes of !quantitative analysis!. A preliminary qualitative examination is generally indispensable, if intelligent and proper provisions are to be made for the separation of the various constituents under such conditions as will insure accurate quantitative estimations.
It is assumed that the operations of qualitative analysis are familiar to the student, who will find that the reactions made use of in quantitative processes are frequently the same as those employed in qualitative analyses with respect to both precipitation and systematic separation from interfering substances; but it should be noted that the conditions must now be regulated with greater care, and in such a manner as to insure the most complete separation possible. For example, in the qualitative detection of sulphates by precipitation as barium sulphate from acid solution it is not necessary, in most instances, to take into account the solubility of the sulphate in hydrochloric acid, while in the quantitative determination of sulphates by this reaction this solubility becomes an important consideration. The operations of qualitative analysis are, therefore, the more accurate the nearer they are made to conform to quantitative conditions.
The methods of quantitative analysis are subdivided, according to their nature, into those of !gravimetric analysis, volumetric analysis!, and !colorimetric analysis!. In !gravimetric! processes the constituent to be determined is sometimes isolated in elementary form, but more commonly in the form of some compound possessing a well-established and definite composition, which can be readily and completely separated, and weighed either directly or after ignition. From the weight of this substance