分析化學與儀器分析

授課教師: 吳 逸 謨 教授
PPT files can be used only in classroom

Introduction to
Analytical Chemistry

Edited from textbook of “Fundamentals of

Analytical Chemistry”
Editors: Skoog, West, Holler, Crouch
Warning: This PPT file is used only in class

Chapter 1 - Introduction
What is Analytical Chemistry?
分析化學 – classical 化學分析
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 What is Analytical Chemistry?

Analytical chemistry is a measurement

science consisting of a set of powerful
ideas and methods that are useful in all
fields of science and medicine.

More detailed definition of “analytical

chemistry” is in following page:

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 Analytical chemistry
Analytical chemistry is the study of the separation, identification, and
quantification of the chemical components of natural and artificial materials.[1]
Qualitative analysis gives an indication of the identity of the chemical species in
the sample, and quantitative analysis determines the amount of certain
components in the substance.
The separation of components is often performed prior to analysis.

Analytical methods can be separated into classical and instrumental.[2]

Classical methods (also known as wet chemistry methods) use separations

such as precipitation, extraction, and distillation and qualitative analysis by color,
odor, or melting point.
Classical quantitative analysis is achieved by measurement of weight or volume.
[Note: It is called “wet chemistry” since most analyzing is done in the liquid phase.]

Instrumental methods use an apparatus to measure physical quantities of the

analyte such as light absorption, fluorescence, or conductivity.

The separation of materials is accomplished using chromatography,

electrophoresis or field flow fractionation methods.

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 Qualitative Analysis vs.
Quantitative Analysis
• Qualitative analysis reveals the identity of
the elements and compounds in a sample.
• Quantitative analysis indicates the amount
of each substance in a sample.

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 Qualitative analysis

A qualitative analysis determines the presence or absence of a particular

compound, but not the mass or concentration. By definition, qualitative analyses
do not measure quantity.

Chemical tests

There are numerous qualitative chemical tests, for example, the acid test for
gold and the Kastle-Meyer test for the presence of blood.
Blood test Kastle-Meyer test - A drop of
Flame/color test
phenolphthalin reagent is added to the
sample.

The presence of copper in this

qualitative analysis is indicated by the
bluish-green color of the flame.
Yellow flame for Na.

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 Analytical Chemistry vs. Instrumental
Analysis
Analytical chemistry is the study of the separation, identification, and
quantification of the chemical components of natural and artificial materials.[1]
Qualitative analysis gives an indication of the identity of the chemical species in
the sample, and quantitative analysis determines the amount of certain
components in the substance.
The separation of components is often performed prior to analysis.

Classical quantitative analysis is achieved by measurement of weight or

volume. Instrumental methods use an apparatus to measure physical
quantities of the analyte such as light absorption, fluorescence, or conductivity.
The separation of materials is accomplished using chromatography,
electrophoresis or field flow fractionation methods.

Analytical chemistry is also focused on improvements in experimental

design, chemometrics, and the creation of new measurement tools to
provide better chemical information.

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 Classical Analytical Chem.
 Modern Instrumentation

Although modern analytical chemistry is dominated by

sophisticated instrumentation, the roots of analytical
chemistry and some of the principles used in modern
instruments are from traditional techniques many of which
are still used today.

These techniques (traditional) also tend to form the

backbone of most undergraduate analytical chemistry
educational labs.

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 1A The Role of Analytical Chemistry
• Analytical chemistry is applied throughout industry,
medicine, and all the sciences.
• Quantitative analytical measurements also play a vital
role in chemistry, biochemistry, biology, geology,
physics, and the other sciences.
• Many scientists devote much time in the laboratory
gathering quantitative information about systems that
are important and interesting to them.

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 1A The Role of Analytical Chemistry

Figure 1-1
The relationship between
analytical chemistry, other
branches of chemistry, and the
other sciences.
The central location of
analytical chemistry in the
diagram signifies its
importance and the breadth of
its interactions with many
other disciplines.

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 1B Classifying Quantitative
Analytical Methods
The results of a typical quantitative analysis are
computed from two measurements:
1. One is the mass or the volume of sample to be
analyzed.
2. The second is the measurement of some
quantity that is proportional to the amount of
analyte in the sample, such as mass, volume,
intensity of light, or electrical charge.

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 1B Classifying Quantitative
Analytical Methods
We classify analytical methods (quantitative) according
to the nature of this final measurement.
1. Gravimetric methods determine the mass of the
analyte or some compound chemically related to
it.
2. Volumetric method determines the volume of a
solution containing sufficient reagent to react
completely with the analyte.

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 1B Classifying Quantitative
Analytical Methods (cont.)
3. Electroanalytical methods involve the
measurement of such electrical properties as
voltage, current, resistance, and quantity of
electrical charge.
4. Spectroscopic methods are based on
measurement of the interaction between
electromagnetic radiation and analyte atoms
or molecules or on the production of such
radiation by analytes.
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 1B Classifying Quantitative
Analytical Methods (cont.)
Miscellaneous methods:
– mass-to-charge ratio
– rate of radioactive decay
– heat of reaction
– rate of reaction
– sample thermal conductivity
– optical activity
– refractive index.

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 Flow Diagram Showing the Steps in a
Quantitative Analysis

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 1C-1 Picking a Method
• One of the first questions to be considered in
the selection process is the level of accuracy
required.
• A second consideration related to economic
factors is the number of samples to be
analyzed.
• The complexity of the sample and the number
of components in the sample always influence
the choice of method to some degree.
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 1C-2 Acquiring the Sample
• Sampling involves obtaining a small mass of a
material whose composition accurately
represents the bulk of the material being
sampled.
• Sampling is frequently the most difficult step in
an analysis and the source of greatest error.
The final results of an analysis will never be
any more reliable than the reliability of the
sampling step.
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 1C-2 Acquiring the Sample
• A material is heterogeneous if its constituent
parts can be distinguished visually or with the
aid of a microscope.
• An assay (化驗,分析) is the process of determining
how much of a given sample is the material
indicated by its name.
• We analyze samples and we determine
substances.

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 1C-3 Processing the Sample
• Under certain circumstances, no sample
processing is required prior to the measurement
step.
• Under most circumstances, we must process the
sample in any of a variety of different ways.
• The first step in processing the sample is often
the preparation of a laboratory sample.

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 1C-3 Processing the Sample
• Preparing a Laboratory Sample
– A solid sample is ground, mixed to ensure
homogeneity, and stored for various lengths of time
before analysis begins.
– Because any loss or gain of water changes the
chemical composition of solids, it is a good idea to
dry samples just before starting an analysis.
– Alternatively, the moisture content of the sample
can be determined at the time of the analysis in a
separate analytical procedure.
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 1C-3 Processing the Sample
• Preparing a Laboratory Sample (Cont.)
– Liquid samples are subject to solvent evaporation
– If the analyte is a gas dissolved in a liquid, analyte
must be kept inside a second sealed container to
prevent contamination by atmospheric gases.
– Extraordinary measures, including sample
manipulation and measurement in an inert
atmosphere, may be required to preserve the
integrity of the sample.

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 1C-3 Processing the Sample
• Replicate samples, or replicates, are portions of a
material of approximately the same size that are
carried through an analytical procedure at the same
time and in the same way.
• Replication improves the quality of the results and
provides a measure of their reliability.
• Quantitative measurements on replicates are
usually averaged, and various statistical tests are
performed on the results to establish their reliability.

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 1C-3 Processing the Sample
• Preparing Solutions: Physical and Chemical Changes
– Ideally, the solvent should dissolve the entire sample,
including the analyte, rapidly and completely.
– The sample may require heating with aqueous solutions
of strong acids, strong bases, oxidizing agents, reducing
agents, or some combination of such reagents.
– It may be necessary to ignite the sample in air or oxygen
or perform a high-temperature fusion of the sample in
the presence of various fluxes.

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 1C-4 Eliminating Interferences
• Few chemical or physical properties of importance
in chemical analysis are unique to a single chemical
species.
• Species other than the analyte that affect the final
measurement are called interferences, or
interferents.
• An interference is a species that causes an error in
an analysis by enhancing or attenuating (making
smaller) the quantity being measured.

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 1C-4 Eliminating Interferences
• Techniques or reactions that work for only one
analyte are said to be specific. Techniques or
reactions that apply for only a few analytes are
selective.
• The matrix, or sample matrix, is all of the
components in the sample containing an
analyte. [note: In chemical analysis, matrix refers to the components
of a sample other than the analyte[1] of interest.]

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 Remain Steps of A Typical
Quantitative Analysis
• 1C-5 Calibration and Measurement
– Ideally, the measurement of the property is directly
proportional to the concentration.
C A = kX
where k is a proportionality constant
• 1C-6 Calculating Results
– Computing analyte concentrations are based on the raw
experimental data collected in the measurement step, the
characteristics of the measurement instruments, and the
stoichiometry of the analytical reaction.

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 Remain Steps of A Typical
Quantitative Analysis
• 1C-7 Evaluating Results by Estimating Their
Reliability
– Analytical results are incomplete without an
estimate of their reliability.

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 1D An Integral Role For Chemical Analysis:
Feedback Control Systems
• Chemical analysis is the measurement element
in all of these examples and in many other
cases.
• The process of continuous measurement and
control is often referred to as a feedback
system, and the cycle of measurement,
comparison, and control is called a feedback
loop [see next page].

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 Feedback Control Systems
Figure 1-3 Feedback system flow
diagram. The desired state is determined,
the actual state of the system is
measured, and the two states are
compared. The difference between the
two states is used to change a
controllable quantity that results in a
change in the state of the system.
Quantitative measurements are again
performed on the system, and the
comparison is repeated. The new
difference between the desired state and
the actual state is again used to change
the state of the system if necessary. The
process provides continuous monitoring
and feedback to maintain the
controllable quantity, and thus the actual
state, at the proper level. The text
describes the monitoring and control of
blood glucose as an example of a
feedback control system.

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 THE END –Chap 1 - Introduction

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