Lecture 1.
Introduction to Analytical Chemistry
INSTRUCTOR: THU VO
What is Analytical Chemistry?
The word analysis comes from the Ancient Greek verb άναλύω
meaning to clarify, to unravel, to unveil a mystery, which is based
on the words άνά (completely) and λύω (to release, to free).
What is Analytical Chemistry?
Determination of the effectiveness of emission-control devices.
Quantities of hydrocarbons, nitrogen oxides, and carbon monoxide present in automobile exhaust
gases are measured.
What is Analytical Chemistry?
• Diagnosis of parathyroid disease in human: quantitative
measurements of ionized calcium in blood serum.
• Nutritional value: Quantitative determination of nitrogen
in foods establishes their protein content.
• Farmers tailor fertilization and irrigation schedules to
meet changing plant needs during the growing season,
gauging these needs from quantitative analyses of
plants and soil.
What is Analytical Chemistry?
“Analytical chemistry is what analytical chemists do.” C. N. Reilley (1925–1981).
In common
• Analytical chemistry is often described as the area of chemistry responsible for
characterizing the composition of matter, both qualitatively and quantitatively.
• Measuring the chemical composition of natural and artificial materials.
• Identify the substances which may be present in a material and determine the exact amounts of
the identified substances.
• Deals with separation, identification, and determination of a component in a sample.
What is Analytical Chemistry?
However,
• Not only in performing a routine analysis on a routine sample (appropriately
called chemical analysis)
… but in improving established methods, extending existing methods to new types
of samples, and developing new methods for measuring chemical phenomena.
What is Analytical Chemistry?
• A more appropriate description
Analytical chemistry is the science of inventing and applying the concepts,
principles, and strategies for measuring the characteristics of chemical systems
and species.
• Analytical chemists typically operate at the extreme edges of analysis, extending
and improving the ability of all chemists to make meaningful measurements on
✓ Smaller samples
✓ More complex samples
✓ Shorter time scales
✓ Species present at lower concentrations.
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.
Applications of Analytical Chemistry
• Analytical chemistry has provided many of the tools
and methods necessary for
• Research in the other four traditional areas of chemistry
• Fostering multidisciplinary research in (medicinal chemistry,
clinical chemistry, toxicology, forensic chemistry, material
science, geochemistry, and environmental chemistry).
Qualitative and Quantitative Analysis
• What substances are contained in a chocolate bar?
• Fat or lipid: saturated or unsaturated?
• Sugar or carbohydrate: glucose, sucrose?
• Cocoa mass or protein
• Micro ingredients: mineral, vitamin, caffeine,…
Qualitative Analysis
• How much of each substance is present in a chocolate bar?
Quantitative Analysis
Qualitative and Quantitative Analysis
• Analytical chemistry can be broken down into two general areas of analysis
• Qualitative analysis: establishes the chemical identity of the species in the sample
• Quantitative analysis: determines the relative amount of these species, or analytes, in
numerical terms.
• Some analytical methods are used primarily for qualitative works, whereas
other methods are mainly quantitative tools. Some methods offer both
information.
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, etc.
Qualitative and Quantitative Analysis
• What substances are contained in a chocolate bar?
• Fat or lipid: saturated or unsaturated?
• Sugar or carbohydrate: glucose, sucrose?
• Cocoa mass or protein
• Micro ingredients: mineral, vitamin, caffeine,…
Qualitative Analysis
• How much of each substance is present in a chocolate bar?
Quantitative Analysis
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.
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.
The Analytical Perspective
1. Identify the problem
Determine type of information 5. Propose a solution
needed(qualitative, quantitative,
characterization, or fundamental) Conduct external evaluation
Identify context of the problem
2. Design the experimental procedure 4. Analyze the experimental data
Establish design criteria (accuracy, Reduce or transform data
precision, scale of operation, Analyze statistics
sensitivity, selectivity, cost,
Verify results
speed)
Feedback Interpret results
Identify interferents
Select method
loop
Establish validation criteria
Establish sampling strategy
3. Conduct an experiment
Calibrate instruments and
equipment
Standardize reagents
Gather data
The Analytical Perspective
• Consider the following questions
1. What is the analytical problem?
2. What type of information is needed to solve the problem?
3. How will the solution to this problem be used?
4. What criteria were considered in designing the experimental procedure?
5. Were there any potential interferences that had to be eliminated? If so, how were they
treated?
6. Is there a plan for validating the experimental method?
7. How were the samples collected?
8. Is there evidence that steps 2, 3, and 4 of the analytical approach are repeated more
than once?
9. Was there a successful conclusion to the problem?
The Analytical Perspective
• Different methods provide a range of precision, sensitivity, selectivity, and
speed capabilities.
The Analytical Perspective
• The essence of analytical chemistry is in the second, third, and fourth steps
of the analytical approach.
• Support broader research goals by developing and validating analytical
methods
• Also define the type and quality of information available to other research
scientists.
• In some cases, the success of an analytical method may even suggest new
research problems.
Common Analytical Problems
• Qualitative analysis
• What is in a sample?
• Quantitative analysis
• The concentration of targeted species in complex samples.
• Characterization analysis
• Physical and chemical properties: chemical structures,
equilibrium constants, particle size, and surface structure, etc.
• Fundamental analysis
• Improving the experimental methods used in other area of
analytical chemistry: extending and improving the theory,
studying a method’s limitations, and designing new and
modifying old methods.
Measurements: SI Units
• SI Units: Systeme International d’Unites
Measurements: SI Units
• SI Units: Systeme International d’Unites
Measurements: SI Units
• SI Units: Systeme International d’Unites
Using prefixes as Multipliers to express large or small quantities.
Measurements: SI Units
• Conversion between SI units and common units.
Solutions and their 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 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏
• Molality: temperature independent
𝒏𝒖𝒎𝒃𝒆𝒓 𝒐𝒇 𝒎𝒐𝒍𝒆 𝒐𝒇 𝒔𝒐𝒍𝒖𝒕𝒆
𝑴𝒐𝒍𝒂𝒍𝒊𝒕𝒚 𝒎 =
𝒌𝒊𝒍𝒐𝒈𝒓𝒂𝒎 𝒐𝒇 𝒔𝒐𝒍𝒗𝒆𝒏𝒕
Solutions and their 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 𝒐𝒓 𝒎𝒊𝒙𝒕𝒖𝒓𝒆
• Parts per Thousand, Parts per Million and Parts per Billion
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒔𝒖𝒃𝒔𝒕𝒂𝒏𝒄𝒆
𝒑𝒑𝒕 = × 𝟏𝟎𝟑
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒔𝒂𝒎𝒑𝒍𝒆
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒔𝒖𝒃𝒔𝒕𝒂𝒏𝒄𝒆
𝒑𝒑𝒎 = × 𝟏𝟎𝟔
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒔𝒂𝒎𝒑𝒍𝒆
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒔𝒖𝒃𝒔𝒕𝒂𝒏𝒄𝒆
𝒑𝒑𝒃 = × 𝟏𝟎𝟗
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒔𝒂𝒎𝒑𝒍𝒆
If considered 1 g or water = 1 mL of water, then:
1 ppt = 1 mg/mL = 1 g/L 1 ppm = 1g/mL = 1 mg/L 1 ppb = 1 ng/mL = 1 g/L
Solutions: Preparing Solution
Solutions: Preparing Solution
• Dilution: Dilute solutions can be prepared from
concentrated solutions.
Measurement: Stoichiometry Calculations
• Stoichiometry is the relationship among the number of moles of reactants and
products as represented by a balanced chemical equation.
• It is derived from the Greek stoicheion (simplest component) and metiri (to
measure).
• Chemical analysis based on weighing a final product is called gravimetric
analysis.
• Gravimetric calculation
aA + bB → cC
𝒂
𝒎𝒐𝒍 𝑨 = 𝒎𝒐𝒍 𝑩
𝒃
𝒃
𝒎𝒐𝒍 𝑩 = 𝒎𝒐𝒍 𝑨
𝒂
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.
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.
Selecting and handling chemical
• Chemical Hazards label
NFPA GHS
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
Electronic analytical balance
Modern analytical chemistry / David Harvey.
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
𝒎′
𝒅𝒘
𝒎=
𝒅
𝟏− 𝒂
𝒅
where da : density of air (0.0012 g/mL near 1 bar and 25 oC)
dw : density of the standard mass (calibration weights, typically 8.0
g/mL)
d : density of the object being weighted.
m : real mass in vacuum
Measuring volume
• Units of volume:
• Liter (L): defined as one cubic decimeter 1 L = 1 dm 3
• 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
• Burette
Volumetric flask
• Used in the diluting of a sample or solution to a certain volume, from 2 L or
more to 1 mL.
• 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.
Modern analytical chemistry, David Harvey.
Volumetric pipets
• Accurately deliver a fixed volume (0.5-200 mL)
• A small volume remains in the tip.
• 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.
Volumetric Pipette One Mark - Class A — SmartLabs
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.
Get 7062 – Mohr Pipettes - Certified Lab Pipettes | Borosil Scientific Class A Graduated Serological Pipette – ISO/DIN-835 Precision
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.
Glassware and Pipetting Flashcards | Quizlet
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.
analytical chemistry - How to identify a blow-out pipette? - Chemistry Stack Exchange
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.
Burette, Acrylic, 50mL - Class B - 0.5mL Blue Graduations - With PTFE — Eisco Labs
Burets
Fundamentals of Analytical Chemistry, Douglas A. Skoog,
Summary
• Analytical chemists work to improve the ability of all chemists to make
meaningful measurements.
• Chemists working in other fields of applied chemistry, as well as the more
traditional areas of chemistry, need better tools for analyzing materials.
• By the time, many requirements challenges analytical chemists to improve
existing analytical methods and to develop new analytical techniques.
• Four typical problems on which analytical chemists work include qualitative
analyses, quantitative analyses, characterization analyses, and fundamental
analyses.
Key terms and References
• Key terms • References
• Fundamentals of Analytical Chemistry, Ninth Edition.
• Characterization analysis
Douglas A. Skoog, Donald M. West, F. James Holler,
• Fundamental analysis Stanley R. Crouch.
• Qualitative analysis • Modern analytical chemistry, First Edition. David Harvey.
• Quantitative analysis • Quantitative Chemical Analysis. Seventh Edition. Daniel C.
Harris.