THE ANALYTICAL ROLE AND PERSPECTIVE Laboratory Grade (LR) Chemicals

Analytical Chemistry - UNILAB found in teaching labs with unknown

impurities.
- measurement of applied science;
- science of inventing and applying concepts of Rules for Chemical Handling
chemistry (Harvey 2000).
1. Select the best grade of chemical available for
Common Analytical Problems: analytical work with small bottle as possible.

1. Qualitative Analysis 2. Replace the top of every container immediately after

- Identifying relative chemical samples. removing reagent.

2. Qualitative analysis 3. Hold the stoppers of reagent bottles between your

- Determining the relative amounts (mass, fingers. Never set a stopper on a desk top.
volume, etc.);
- Vital in research field. 4. Unless specifically directed otherwise, never return
any excess reagent to a bottle.
➢ Gravimetric Methods
- determine the mass of the analyte or compound. 5. Use a clean porcelain in the bottle that contains a
solid chemical unless directed otherwise.
➢ Volumetric Methods
- measure the volume of a solution. 6. Keep the reagent shelf and the laboratory balance
clean and neat. Clean up any spills immediately.
➢ Electroanalytical Methods
- measure electrical properties. 7. Follow local regulations concerning the disposal of
surplus reagents and solutions.
➢ Spectroscopic Methods
- electromagnetic radiation and analyte atoms. Analytical Balance

- measure masses accurately with a maximum

3. Characterization Analysis
capacity that ranges from 1 g to a few kilograms
- analysis in which a sample’s chemical or physical
with a precision of at least 1 part in 105 at
properties are evaluated.
maximum capacity.

4. Fundamental Analysis Types of Analytical Balances

- analysis whose purpose is to improve an
Microbalance
analytical method’s capabilities.
- most common type of analytical balance, and it
TOOLS IN ANALYTICAL CHEMISTRY
has a maximum load of 160 to 200 g and a
Chemicals precision of 0.1 mg.

Reagent Chemicals Semimicro Analytical Balance

- conform to the minimum standards set forth by - Has a maximum load of 10 to 30 g and a precision
the ACS and are used in analytical work in drug of 0.01 mg.
and food.
Microanalytical Balance

- has a maximum load of 1 to 3 g and a precision

Primary-Standard Grade
of 0.001 mg, or 1 μg.
- carefully analyzed by the supplier, and the
Precautions in Using an Analytical Balance:
results are printed on the container label.
(NIST)’s complex substances that have been 1. Center the load on the pan as well as possible.
exhaustively analyzed.
2. Protect the balance from corrosion. Objects to be
Special-Purpose Reagent placed on the pan should be limited to nonreactive
metals, nonreactive plastics, and vitreous, or glasslike,
- Chemicals that have been prepared for a specific
materials.
application.
3. Consult your instructor if the balance appears to need
adjustment.

4. Keep the balance and its case clean. A camel’s-hair

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 5. Always allow an object that has been heated to return *In reading volumes, the eye must be at the level of the
to room temperature before weighing it. liquid*

6. Use tongs, finger pads, or a glassine paper strip to Parallax

handle dried objects to prevent transferring moisture to
- a condition that causes the volume to appear
them.
smaller than its actual value.
Equipment and Manipulations Associated with
Safety in The Laboratory
Weighing
1. Before you begin work in any laboratory, learn the
The mass of many solid changes with humidity.
location of the nearest eye fountain, fire blanket,
*The establishment of constant mass provides some shower, and fire extinguisher. Learn the proper use
assurance that the chemical or physical processes that of each, and do not hesitate to use this equipment
occur during the heating (or ignition) are complete* if the need arises.

Desiccators and Desiccants

2. Wear eye protection at all times. Contact lenses
Oven drying is the most common way of removing should never be used in the laboratory because
moisture from solids. To minimize the uptake of laboratory fumes may react with them and have a
moisture, dried materials are stored in desiccators while harmful effect on the eyes.
they cool.
3. Most of the chemicals in a laboratory are toxic and
Weighing by Difference highly corrosive. Avoid contact between these
- simple method for determining a series of liquids and the skin. In the event of such contact,
sample masses. immediately flood the affected area with large
quantities of water. If a corrosive solution is spilled
*The mass of the sample is the difference between the on clothing, remove the garment immediately.
two masses. It is essential that all the solid removed from
the weighing bottle be transferred without loss to the 4. NEVER perform an unauthorized experiment.
container*

Hygroscopic Substances 5. Never work alone in the laboratory.

- rapidly absorb moisture from the atmosphere 6. Never bring food or beverages into the laboratory.
and require special handling. NEVER drink from laboratory glassware. NEVER
smoke in the laboratory.
Apparatus

- Volumetric equipment is marked by the 7. Always use a bulb or other device to draw liquids
manufacturer to indicate the manner and into a pipet. NEVER pipet by mouth.
temperature of the calibration.
8. Wear adequate foot covering (no sandals). Confine
Pipets (0.5 to 200 mL)
long hair with a net. A laboratory coat or apron will
- permit the transfer of accurately known volumes provide some protection and may be required.
from one container to another.
9. Be extremely tentative in touching objects that
have been heated because hot glass looks exactly
Volumetric Flasks (5 mL to 5 L) like cold glass.
- are usually calibrated to contain (TC) a specified
volume. 10. Use fume hoods whenever toxic or noxious gases
- Used for the preparation of standard solutions are likely to be evolved. Be cautious in testing for
and for the dilution of samples to a fixed volume. odors. Use your hand to waft vapors above
containers toward your nose.
Burets

- make it possible to deliver any volume up to the 11. Notify your instructor immediately in the event of
maximum capacity of the device. an injury.
- precision attainable is substantially greater than
the precision with a pipet. 12. Dispose of solutions and chemicals as instructed. It
is illegal to flush solutions containing heavy metal
Meniscus ions or organic liquids down the drain in most
- The top surface of a liquid confined in a narrow localities.
tube exhibits a marked curvature.
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 CHEMICAL STOICHIOMETRY Mole Method

Stoichiometry - the stoichiometric coefficients in a chemical

equation can be interpreted as the number of
- is the study that examines the quantities of moles of each substance.
substances consumed and produced in chemical
reactions SOLUTION STOICHIOMETRY
- law of conservation of mass.
Concentration
Chemicals Equations
- the amount of solute dissolved in a given
- represent chemical reactions. quantity of solvent or quantity of solution.

Reactants *The greater the amount of solute dissolved in a certain

- The chemical formulas to the left are the starting amount of solvent, the more concentrated the resulting
substances.
solution*
Products
Molarity (M)
- The chemical formulas to the right are the
- expresses the concentration of a solution as the
substances produced in the reaction.
number of moles of solute in a liter of solution.
Coefficients - M= mol/L

- relative numbers of molecules of each kind Stock Solutions

involved in the reaction.
- concentrated form of solutions used routinely in
Chemical Equations the laboratory.

- The number of atoms is obtained by multiplying Dilution

each subscript in a chemical formula by the
- Solutions of lower concentrations can then be
coefficient for the formula.
obtained by adding water.
Balancing Equations
CHEMICAL EQUILIBRIUM
Never change subscripts when balancing an equation. In
contrast, placing a coefficient in front of a formula Chemical Equilibrium
changes only the amount of the substance and not its - occurs when opposing reactions proceed at
identity. equal rates: The rate at which the products form
Molar Mass from the reactants equals the rate at which the
reactants form from the products.
- mass in grams per mole (g/mol) of the substance.
Equilibrium Constant
Empirical formula
- A reaction in which reactants convert to
- the relative number of atoms of each element in products and products convert to reactants in
the substance. the same reaction vessel naturally leads to an
Limiting reactants equilibrium.

- The reactant that is completely consumed in a Le Châtelier’s Principle

reaction. - If a system at equilibrium is disturbed by a
- determines, or limits, the amount of product change in temperature, pressure, or a
formed. component concentration, the system will shift
Theoretical Yields its equilibrium position so as to counteract the
effect of the disturbance.
- The quantity of product calculated to form when
all of a limiting reactant is consumed.

Actual yield

- the amount of product actually obtained and

almost always less than the theoretical yield.

Percent yield

- relates actual and theoretical yields.

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 THE LANGUAGE OF ANALYTICAL CHEMISTRY 2. Precision
- indication of the reproducibility of a
Analysis measurement or result.
- process that provides chemical or physical
information about the constituents. 3. Sensitivity
- measure of a method’s ability to distinguish
Analytes between two samples.
- the constituents of interest in a sample.
4. Robust
Matrix - method that can be applied to analytes in a wide
variety of matrices is considered robust.
- all other constituents in a sample except for the
analytes.
5. Rugged
Technique - method that is insensitive to changes in
experimental conditions is considered rugged.
- chemical or physical principle that can be used to
analyze a sample. Calibration
Method - ensures that the equipment or instrument used
to measure the signal is operating correctly by
- application of a technique for the determination
using a standard known to produce an exact
of a specific analyte in a specific matrix
signal.
Procedure
Validation
- a set of written directions detailing how to apply
- the process of verifying that a procedure yields
a method to a particular sample
acceptable results.
Protocol
Quality Assurance and Quality Control (QA/QC)
- a set of stringent written guidelines detailing the
- those steps taken to ensure that the work
procedure that must be followed if the agency
conducted in an analytical lab is capable of
specifying the protocol is to accept the results of
producing acceptable results.
the analysis.

APHA = American Public Health Association

ASTM = American Society for Testing Materials

EPA = Environmental Protection Agency

Classifying Analytical Techniques

Signal

- An experimental measurement that is

proportional to the amount of analyte.

1. Total Analysis Techniques

- Techniques responding to the absolute amount
of analyte.

2. Concentration Techniques
- Techniques wherein the signal is proportional to
the relative amount of analyte in a sample.

Selecting an Analytical Method

Design criteria:

1. Accuracy
- a measure of how closely the result of an
experiment agrees with the expected result.
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