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
𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒
𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 (𝑀) =
𝐿𝑖𝑡𝑒𝑟 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡
• Molality: temperature independant
𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒
𝑀𝑜𝑙𝑎𝑙𝑖𝑡𝑦 (𝑚) =
𝑘𝑖𝑙𝑜𝑔𝑟𝑎𝑚 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡
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Measurements: Chemical Concentrations
• Percent Composition:
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒
𝑊𝑒𝑖𝑔ℎ𝑡 𝑝𝑒𝑟𝑐𝑒𝑛𝑡 (𝑤𝑡%) = ×100
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑡𝑜𝑡𝑎𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 𝑜𝑟 𝑚𝑖𝑥𝑡𝑢𝑟𝑒
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒
𝑉𝑜𝑙𝑢𝑚𝑒 𝑝𝑒𝑟𝑐𝑒𝑛𝑡(𝑣𝑜𝑙%) = ×100
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑜𝑡𝑎𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
• Parts per Million and Parts per Billion:
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑢𝑏𝑠𝑡𝑎𝑛𝑐𝑒
𝑝𝑝𝑚 = ×106
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑢𝑏𝑠𝑡𝑎𝑛𝑐𝑒
𝑝𝑝𝑏 = ×109
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
– If considered 1 g of water = 1 mL of water, then:
1 ppm = 1 µg/mL (= 1 mg/L) and 1 ppb = 1ng/mL (=1 µg/L )
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Measurements: Preparing Solution
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Measurements: Preparing Solution
• Dilution:
𝑀EFGE. 𝑉EFGE. = 𝑀IJK. 𝑉IJK .
(Moles taken from (Moles taken from
concentrated solution) diluted solution)
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Measurements: Calculations of Stoichiometry
• Gravimetric calculation
aA + bB à cC
𝑎
𝑚𝑜𝑙 𝐴 = 𝑚𝑜𝑙 𝐵
𝑏
𝑏
𝑚𝑜𝑙 𝐵 = 𝑚𝑜𝑙 𝐴
𝑎
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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 (µL) = 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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