An Introductory Course of Quantitative Chemical Analysis | Page 2

gained the conclusion has been
reached that volumetric analysis offers the better approach to the
subject. Accordingly the arrangement of the present (the sixth) edition
of this manual 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