Analytical Chemistry

Chapter 1
Introduction to Analytical Chemistry

Instructor: Nguyen Thao Trang

What is analytical chemistry?
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• Analytical chemistry seeks improved means of measuring the
chemical composition of natural and artificial materials.

• The techniques of this science are used to identify the

substances which may be present in a material and determine
the exact amounts of the identified substances.

• Is the branch of chemistry that deals with separation,

identification, and determination of a component in a sample.

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The roles of analytical chemistry
• Improve the reliability of existing techniques to meet the
demands of for better chemical measurements which arise
constantly in our society.

• Adapt proven methodologies to new kinds of materials or to

answer new questions about their composition.

• Carry out research to discover completely new principles of

measurements and are at the forefront of the utilization of
major discoveries such as lasers and microchip devices for
practical purposes.

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The roles of analytical chemistry

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Fundamentals of analytical chemistry, Skoog, D. A
Quantitative and qualitative analysis
• Can be broken down into two general areas of analysis:

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Fundamentals of analytical chemistry, Skoog, D. A
Analytical chemistry
• Can be broken down into two general areas of analysis:

– Qualitative analysis: Determination of what materials present in a

sample

– Quantitative analysis: Determination of how much a material is

present in a sample

• Some analytical methods are used primarily for qualitative

works, whereas other methods are mainly quantitative tools.
Some methods offer both information.

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Classification of analytical methods
• Gravimetric methods

• Volumetric methods

• Electroanalytical methods

• Spectroscopic methods

• Miscellaneous: measure such quantities as mass-to-charge

ratio, heat of reaction, rate of reaction,…

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Qualitative analysis

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Fundamentals of analytical chemistry, Skoog, D. A
Qualitative analysis
• Determination of what materials present in a sample →
identity of an atomic, molecular or biomolecular species.

• Qualitative tests may be performed by:

• Selective chemical reactions: certain chemical reactions will produce
colors or precipitate to indicate the presence of certain compounds.

• Use of instrumentation: Infrared spectra will give "fingerprints"of

organic compounds or their functional groups.

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Quantitative analysis
HOW MUCH CAFFEIN IS IN A CHOCOLATE BAR?

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Quantitative analysis
• Determination of how much a material is present in a sample
→ provides numerical information as to the relative amounts
of species

• Quantitative analysis can be performed by:

• Selective chemical reactions

• Use of instrumentation

• Quantitative analysis is often more complicated than

qualitative analysis.

• Requires calculation of results and estimation of result

reliability.
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General process in analytical chemistry
• General steps in an analysis include:
– Define problem
– Select a method
– Obtain a representative sample
– Prepare the sample for analysis
– Perform any necessary chemical separations
– Perform the measurement
– Calculate the results and report

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General process in analytical chemistry

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Analytical chemistry, Gary Christian.
General process in analytical chemistry

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Analytical chemistry, Gary Christian.
General process in analytical chemistry

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Analytical chemistry, Gary Christian.
General process in analytical chemistry

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Analytical chemistry, Gary Christian.
General process in analytical chemistry

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Analytical chemistry, Gary Christian.
General process in analytical chemistry

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Analytical chemistry, Gary Christian.
General process in analytical chemistry
• Different methods provide a range of precision, sensitivity,
selectivity, and speed capabilities

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Measurements: SI Units
• SI Units: Systeme International d'Unites

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Measurements: SI Units
• SI Units: Systeme International d'Unites

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Measurements: SI Units
• SI Units: Systeme International d'Unites
- Using prefixes as Multipliers to express large or small
quantities.

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Measurements: SI Units
• SI Units: Systeme International d'Unites
- Conversion between SI units and common units.

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Measurements: Chemical Concentrations
• A solution is a homogeneous mixture of two or more
substances:
– Minor species called solute,
– Major species is the solvent.
– Concentration: how much solute is contained in a given volume or
mass of solution or solvent, expressed by molarity or molality.

• Molarity: temperature depending

( )=

• Molality: temperature independant

( )=

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Measurements: Chemical Concentrations
• Percent Composition:

ℎ ( %) = × 100

( %) = × 100

• Parts per Million and Parts per Billion:

= × 106

= × 109

– If considered 1 g of water = 1 mL of water, then:

1 ppm = 1 g/mL (= 1 mg/L) and 1 ppb = 1ng/mL (=1 g/L )
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Measurements: Preparing Solution

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Measurements: Preparing Solution
• Dilution:
. . = . .

(Moles taken from (Moles taken from

concentrated solution) diluted solution)

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Measurements: Calculations of Stoichiometry
• Gravimetric calculation
aA + bB  cC

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Selecting and handling chemical
• Chemical classification:

– Reagent grade: chemicals conform minimum standards stated by

the Reagent Chemical Committee of the American Chemical Society
(ACS) and are used wherever possible in analytical work.

– Primary standard grade: chemicals required extraordinary purity

– Special purpose reagent grade: chemical prepared for a specific

application, as for spectrophotometric and chromatographic use

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Selecting and handling chemical
• Chemical handling:
– Select the best grade of chemical available for analytical work.
Whenever possible, pick the smallest bottle that will supply the
desired quantity.

– Unless specifically directed, never return any excess reagent to a

bottle.

– Keep the reagent shelf and the laboratory balance clean and neat
Clean up any spills immediately, even though someone else is waiting
to use the same chemical or reagent.

– Observe local regulations concerning the disposal or surplus reagents

and solutions.

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Selecting and handling chemical
• Chemical Hazards label:

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Balance
• An analytical balance is an instrument for determining mass
with a maximum capacity that ranges from grams to a few
kilograms with a precision of at least 1 part in 105 at
maximum capacity.

• Type of analytical balances:

– Analytical balance (macrobalance): maximum capacity ranging
between 160-200 g and a standard deviation of ± 0.1 g
– Semi-microanalytical balance: maximum capacity ranging between 20
-30 g and a standard deviation of ± 0.01 g
– Microanalytical balance: maximum capacity ranging between 1 -3 g
and a standard deviation of ± 0.001 g

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Electronic analytical balance

Fig. 2.1. Electronic analytical balance.

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Analytical chemistry, Gary Christian.
Buoyancy
• Buoyancy is the upward force exerted on an object in liquid or
gaseous fluid.
• Weight of an object in air m’ can be corrected to the weight in
vacuum m by:

– da = density of air (0.0012 g/mL near 1 bar and 25oC)

– dw = density of the standard mass (calibration weights, typically 8.0
g/mL)
– d = density of the object being weighed.

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Measuring volume
• Units of volume:
– Liter(L): defined as one cubic decimeter 1 L = 1 dm3
– 1 milliter (mL) = 10-3 L
– 1 microliter (L) = 10-3 mL = 10-6 L
• Effect of temperature on measuring volume
• Apparatus for measuring volume
– Volumetric flask
– Pipet
– Buret

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Volumetric flask
• Used in the diluting of a sample or solution to a certain
volume, from 2 L or more to 1 mL.
• Is designed to contain an accurate volume at the specified
temperature (20 or 25°C) when the bottom of the meniscus
just touches the etched "fill" line across the neck of the glass.

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Analytical chemistry, Gary Christian. Modern analytical chemistry, David Harvey
Volumetric pipets
• Accurately deliver a fixed volume (0.5-200
mL)
• A small volume remains in the tip.
• Is used for accurate measurements since it
is designed to deliver only one volume and
is calibrated at that volume.
• Accuracy to 4-5 significant figures is
generally achieved.

Analytical chemistry, Gary Christian.

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Measuring pipets
• Measuring (or graduated) pipets accurately deliver variable
volumes (0.1-25 mL).
• Measuring pipettes are divided into:
– MOHR PIPET: the graduations always end before the tip.

– SEROLOGICAL PIPET: the graduation marks continue to the

tip

• A small volume remains in the tip or has to be blown out.

• Less accurate than volumetric pipets.

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Measuring pipets
• Specification on measuring pipet:

– the maximum volume of liquid that can be transferred

– the size of the divisions on the pipette

– the temperature at which calibrations were made

– if the pipette is a “to deliver”(TD) or “to contain”(TC) pipette.

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Measuring pipets
• “To blow out” a serological pipet if:
– has a frosted band or two thin rings around the neck.
– This means that after all the liquid has been allowed to drain out by
gravity, the last drop remaining in the tip is also forced out.

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Burets
• Possible to deliver any volume up to the
maximum capacity of the device
• Its principal use is in titrations.
• The conventional buret for
macrotitrations is marked in 0.1 mL
increments from 0 to 50 mL.
• Deliver at a fairly slow rate, about 15-20
mL/min. Near the end point, the rate of
delivery is only a few drops per minute
• Two readings are taken for every volume
measurement.

Analytical chemistry, Gary Christian.

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Burets

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