Analytical Chemistry 602027-Chapter 1

7/16/2020
TON DUC THANG UNIVERSITY

Faculty of Applied Sciences
7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 1
BRIEF COURSE CONTENT
• Introduction to analytical chemistry

• Classical analytical methods: volumetric and weight analysis
• Instrumental methods: chromatography, photospectroscopy, and
electrochemistry
Course learning outcomes (CLOs):

• Remember all definitions, parameters, tools, instruments, and formulas
related to analytical chemistry; remember the principles of each method, the
preparation between modern and classical methods of analytical chemistry.
• Understand the objectives of each analytical method, understand all steps of
specific procedure, understand the differences between various analytical
techniques
• Apply correctly the analytical methods for specific samples / compounds with
various contents / components
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COURSE PROGRAMME
Evaluation of this course

Evaluation categories Weight (%) Types of questions
Formative evaluation 1 10 Process Exercise
Formative evaluation 2 20 Process Exercise
Mid-term test 20 Multiple choice question
Final examination 50 Multiple choice question
References
[1]. Daniel C.Harris, [2007], Quantitative chemical analysis, 7th ed., W. H. Freeman and Company, New York.
[2]. Kreskov (author); Tu Vong Nghi, Tran Tu Mieu (translator), [1990], Co so & hoa hoc phan tich - tap 2,
NXB dai hoc va giao duc chuyen nghiep, Hanoi, VN.
[3]. Douglas A. Skoog, et al., [2014], Fundamentals of analytical chemistry, 8th ed., Brooks/Cole - Thomson
Learning, Belmont.
[4]. Makoto (author); Tran Thi Ngoc Lan (translator), [2006], Cac phuong phap phan tich trong hoa hoc, NXB
Kagaku, Kyoto.
[5]. Hoang Minh Chau, Tu Van Mac, Tu Vong Nghi, [2002], Co so Hoa hoc Phan tich, NXB Khoa hoc va Ky
thuat, Ha Noi, Vietnam.
Chapter 1:
Introduction to analytical chemistry
1.1. General introduction of analytical chemistry

1.2. Measurements and tools in analytical chemistry
1.3. Number, significant digit and error
1.4. Analytical methods
1.5. Sample preparation
1.6. Statistical methods in quantification
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Chapter 1:
1.1. General introduction of

analytical chemistry
- Analytical chemistry: a
measurement science
• a set of powerful ideas and

methods
• in all fields of science,

engineering, and medicine
Chapter 1:
1.1. General introduction of analytical chemistry

- Quantitative analysis determines the
relative amounts of these species, or
analytes, in numerical terms.
- Qualitative analysis is often an integral

part of the separation step, and determining
the identity of the analytes is an essential
adjunct to quantitative analysis.
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Chapter 1:
1.1. General introduction of

analytical chemistry
• gravimetric methods
• volumetric method
The steps in a quantitative analysis
Chapter 1:

Classifying Chemicals
- Reagent Grade
- Primary-Standard Grade
- Special-Purpose Reagent Chemicals
Rules for Handling Reagents and Solutions
1. Select the best grade of chemical available for analytical work.
Whenever possible, pick the smallest bottle that is sufficient to do the
job.
2. Replace the top of every container immediately after removing
reagent. Do not rely on someone else to do so.
3. Hold the stoppers of reagent bottles between your fingers. Never set a
stopper on a desk top.
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Chapter 1:

Rules for Handling Reagents and Solutions (cont.)
5. Unless directed otherwise, never insert spatulas, spoons, or knives
into a bottle that contains a solid chemical. Instead, shake the capped
bottle vigorously or tap it gently against a wooden table to break up an
encrustation. Then pour out the desired quantity. These measures are
occasionally ineffective, and in such cases a clean porcelain spoon
should be used.
6. Keep the reagent shelf and the laboratory balance clean and neat.
Clean up any spills immediately.
7. Follow local regulations concerning the disposal of surplus reagents
and solutions.
Chapter 1:

Measuring mass Precautions in Using an Analytical Balance
1. Center the load on the pan as well as possible.
2. Protect the balance from corrosion. Objects to be placed on
the pan should be limited to nonreactive metals, nonreactive
plastics, and vitreous, or glasslike, materials.
3. Observe special precautions for the weighing of liquids.
4. Consult your instructor if the balance appears to need
adjustment.
5. Keep the balance and its case scrupulously clean. A camel’s-
hair brush is useful for removing spilled material or dust.
6. Always allow an object that has been heated to return to room
temperature before weighing it.
7. Use tongs, finger pads, or a glassine paper strip to handle
dried objects to prevent transferring moisture to them.
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Chapter 1:

Measuring mass
• Auxiliary Balances
• Use auxiliary laboratory balances for determining masses

that do not require great accuracy.
• Example:
150 to 200 g with a precision of about 1 mg
25,000 g with a precision of 60.05 g
Chapter 1:

A typical desiccator
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Chapter 1:

Vacuum filtration Filter paper folding
Chapter 1:
Apparatus
for precisely
measuring
volume
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Chapter 1:

Apparatus for precisely measuring volume
Chapter 1:

Apparatus for precisely
measuring volume
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Chapter 1:

Reading a buret.
(a) The student reads the buret from a position
above a line perpendicular to the buret and makes
a reading
(b) of 12.58 mL. (c) The student reads the buret
from a position along a line perpendicular to the
buret and makes a reading (d) of 12.62 mL. (e)
The student reads the buret from a position below
a line perpendicular to the buret and makes a
reading (f) of 12.67 mL.
To avoid the problem of parallax, buret readings
should be made consistently along a line
perpendicular to the buret, as shown in (c) and (d).
Chapter 1:

a rubber bulb (B)
a small chemically inert ball (A, C, and D): a valve to
permit air to flow normally in the directions indicated
by the arrows. The valves are opened by pinching
with a thumb and forefinger. The bottom of the device
fits snugly on the top of a pipet. Operation begins by
opening valve A and squeezing bulb B to expel the air
in the bulb. Valve A is then closed, and valve C is
opened to draw liquid into the pipet to the desired
level, after which C is closed. The liquid level is then
adjusted in the pipet by carefully opening valve D,
and finally, the liquid in the pipet is delivered by
opening valve D completely.
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Chapter 1:
Chapter 1:
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Chapter 1:
Chapter 1:

• The significant figures in a number
are all of the certain digits plus the first
uncertain digit.
rules for determining the
number of significant figures:
1. Disregard all initial zeros.
2. Disregard all final zeros unless they follow a
decimal point.
3. all remaining digits including zeros between
nonzero digits are significant.
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Chapter 1:

• Significant Figures in Numerical Computations
Sums and Differences
As a rule of thumb, for addition and subtraction, the result

should contain the same number of decimal places as the
number with the smallest number of decimal places.
Chapter 1:

Products and Quotients
Express the numbers to the same power of ten
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Chapter 1:

Products and Quotients
The comparison of the relative uncertainties associated with

each of these numbers: 1/24 > 1/452 > 1/1000
The absolute uncertainty:
Chapter 1:

Logarithms and Antilogarithms
1. In a logarithm of a number, keep as many digits to the
right of the decimal point as there are significant figures
in the original number.
2. In an antilogarithm of a number, keep as many digits
as there are digits to the right of the decimal point in the
original number.
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Chapter 1:

• Rounding Data
In rounding a number ending in 5, always round so that
the result ends with an even number. thus,
0.635 rounds to 0.64 and
0.625 rounds to 0.62.
Keep two significant figures of the standard deviation in

research articles, we should note that it is seldom
justifiable to keep more than one significant figure in the
standard deviation.
Chapter 1:
• Expressing Results of Chemical Calculations

It is especially important to postpone rounding until the
calculation is completed.
At least one extra digit beyond the significant digits should be
carried through all of the computations in order to avoid a
rounding error. This extra digit is sometimes called a “guard”
digit.
There is no relationship between the number of digits
displayed on a computer screen or a calculator and the true
number of significant figures.
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Chapter 1:
Chapter 1:

The mean: the arithmetic mean or the average
The deviation from the mean di
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Chapter 1:

Sources of Systematic Errors
Instrumental errors are caused by nonideal instrument
behavior, by faulty calibrations, or by use under
inappropriate conditions.
Method errors arise from nonideal chemical or physical
behavior of analytical systems.
Personal errors result from the carelessness, inattention, or
personal limitations of the experimenter
Bias measures the systematic error associated with an analysis. It has a
negative sign if it causes the results to be low and a positive sign otherwise.
Chapter 1:
Constant errors are independent of the size of the

sample being analyzed.
Proportional errors decrease or increase in

proportion to the size of the sample.
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Chapter 1:

• Detection of Systematic Method Errors
Standard reference materials (SRMs)
are substances sold by the National Institute of Standards
and Technology (NIST) and certified to contain specified
concentrations of one or more analytes.
Independent Analysis: If standard samples are not available,
a second independent and reliable analytical method can be
used in parallel with the method being evaluated.
Chapter 1:
• Blank Determinations
A blank solution contains the solvent and all of the
reagents in an analysis. Whenever feasible, blanks
may also contain added constituents to simulate
the sample matrix.
The term matrix refers to the collection of all the
constituents in the sample.
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Chapter 1:

• The nature of random error:
Random, or indeterminate, errors can never be totally
eliminated and are often the major source of uncertainty
in a determination. Random errors are caused by the
many uncontrollable variables that accompany every
measurement.
It is often impossible to measure random errors
because most are so small that they cannot be detected
individually.
All the uncertainties have the same magnitude, this
restriction is not necessary to derive the equation for a
Gaussian curve.
Chapter 1:

- Distinguish a method of identifying chemical species, a
qualitative analysis, from one to determine the amount
of a constituent, a quantitative analysis.
- Sample Size
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Chapter 1:

Classification of analyses by sample size
Chapter 1:

- Constituent Types
analytical methods are used to determine major
constituents, which are those present in the range of 1 to
100% by mass
species present in the range of 0.01 to 1% are usually
termed minor constituents
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Chapter 1:

Classification of constituent types by analyte level.
Chapter 1:

Samples are analyzed, but constituents or concentrations
are determined.
Sampling is often the most difficult aspect of an analysis.
The process by which a representative fraction is acquired is
termed sampling.
In sampling, a sample population is reduced in size to an
amount of homogeneous material that can be conveniently
handled in the laboratory and whose composition is
representative of the population.
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Chapter 1:
Steps in obtaining a laboratory

sample. The laboratory sample
consists of a few grams to at most a
few hundred grams. It may
constitute as little as 1 part in 107 or
108 of the bulk material.
Chapter 1:

Statistically, the goals of the sampling process are:
1. To obtain a mean analyte concentration that is an unbiased
estimate of the population mean. This goal can be realized
only if all members of the population have an equal probability
of being included in the sample.
2. To obtain a variance in the measured analyte concentration
that is an unbiased estimate of the population variance so that
valid confidence limits can be found for the mean, and various
hypothesis tests can be applied. This goal can be reached only
if every possible sample is equally likely to be drawn.
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Chapter 1:

• The gross sample is the collection of individual
sampling units. It must be representative of the
whole in composition and in particle-size
distribution.
• The number of particles required in a gross sample
ranges from a few particles to 1012 particles.
• To simplify the problem of defining the mass of a
gross sample of a multicomponent mixture, assume
that the sample is a hypothetical two-component
mixture.
Chapter 1:

Steps in sampling a particulate solid
• Sampling Homogeneous Solutions of Liquids

and Gases
Well-mixed solutions of liquids and gases
require only a very small sample because they
are homogeneous down to the molecular level.
• Sampling Particulate Solids (Mechanical devices
have been developed for handling many types of
particulate matter)
• Sampling Metals and Alloys: obtained by
sawing, milling, or drilling
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Chapter 1:
Chapter 1:
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Chapter 1:
Chapter 1:
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Chapter 1:
Chapter 1:

Example:
A clinical chemist obtained the following data for the
alcohol content of a sample of blood: % C2H5OH: 0.084,
0.089, and 0.079. Calculate the 95% confidence interval
for the mean assuming that (a) the three results obtained
are the only indication of the precision of the method
and that (b), from previous experience on hundreds of
samples, we know that the standard deviation of the
method s = 0.005% C2H5OH and is a good estimate of
.
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Chapter 1:

Example: (solution)
26

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7/16/2020

TON DUC THANG UNIVERSITY

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 1

BRIEF COURSE CONTENT

• Introduction to analytical chemistry

Course learning outcomes (CLOs):

Evaluation of this course

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 3

1.1. General introduction of analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 4

1.1. General introduction of

• a set of powerful ideas and

• in all fields of science,

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 5

1.1. General introduction of analytical chemistry

- Qualitative analysis is often an integral

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 6

1.1. General introduction of

The steps in a quantitative analysis

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 7

1.2. Measurements and tools in analytical chemistry

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 9

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 10

1.2. Measurements and tools in analytical chemistry

• Use auxiliary laboratory balances for determining masses

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 11

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 12

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 13

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 14

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 15

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 16

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 17

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 18

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 19

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 20

1.2. Measurements and tools in analytical chemistry

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 21

1.3. Number, significant digit and error

1.3. Number, significant digit and error

As a rule of thumb, for addition and subtraction, the result

1.3. Number, significant digit and error

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 24

1.3. Number, significant digit and error

The comparison of the relative uncertainties associated with

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 25

1.3. Number, significant digit and error

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 26

1.3. Number, significant digit and error

Keep two significant figures of the standard deviation in

1.3. Number, significant digit and error

• Expressing Results of Chemical Calculations

7/16/2020 602027 – Chapter 1: Introduction to analytical chemistry 28

1.3. Number, significant digit and error