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Analytical CHEM Reviewer

Analytical Chemistry (Our Lady of Fatima University)

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ANALYTICAL CHEM Order sample, preparation, carry out analysis, work data and
calculate and report the result.
Intro and Lab math

Analytical Science

• The science that deals with the identification and

quantification of the components of material systems

• Analysis - the process of determining the level of any or

all components in a material system

Analytical Chemistry

• A BRANCH OF CHEMISTRY THAT DEALS WITH THE

SEPARATION, IDENTIFICATION AND QUANTIFICATION
OF CHEMICAL COMPOUNDS

• QUALITATIVE AND QUANTITATIVE ANALYSIS

o QUALITATIVE ANALYSIS- An analysis that
establishes the chemical identity of the species
o Quantitative Analysis - An analysis that
determines the relative amounts of analytes in
numerical term

Analytical Strategy

• The process involving many individual steps by which an

analyte’s identity or concentration in a sample is
determined

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Fundamental Units of Measurement Scientific Notation

• SI units • A numerical system in which numbers are expressed in

o Standardized system of units adapted by the form A x 10n
scientists throughout the world • where A is a number with a single nonzero digit to the
left of the decimal place and n is a whole number
• The exponent for the exponential term is equal to the
number of places the decimal point has been moved
o Positive (+) n means a large number so the
decimal moves to the right by n places.
o Negative (-) n means a small number so the
decimal moves to the left by n places.

Scientific Notation

• When converting from standard notation to scientific

notation
o If the number is one or greater you will have a
positive exponent and move the decimal to the
left.

• Prefixes for Units

o If the number is less than one you will have a

negative exponent and move the decimal to the
right.

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o # Of spaces moved by decimal = exponent o Zeros at the end of a number are SIGNIFICANT if a
decimal point is PRESENT in the number
o If the exponent is positive, you will have a large ▪ Ex. 56.00 has four significant figures
number (>1) and move the decimal to the right. ▪ 0.05050 has four significant figures
o Zeros at the end of a number are NOT
SIGNIFICANT in the number LACKS an explicitly
shown decimal point
▪ Ex. 59,000,000 has two significant figures
▪ 6010 has three significant figures
o If the exponent is negative, you will have a small
number (<1) and move the decimal to the left
Solution Properties

• A substance that is dissolved in a liquid is called a solute

• The liquid in which the solute is dissolved is the solvent
• Together they represent a solution
Significant figures

• In measurements there is always some amount of Molarity

uncertainty.
• Molarity (M) is expressed as the number of moles per 1 L
1. All nonzero digits are significant of solution.
2. Zeros may or may not be significant • A solution that is 1.0 M contains 1.0 mole of solute per
o Zeros at the beginning of a number are never liter of solution
significant • Molarity Formula
▪ Ex. 0.0141 has three significant figures
o Zeros between nonzero digits are always
significant
▪ Ex. 3.063 has four significant figures
▪ 0.001004 has four significant figures

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Molality Percent solutions

• Molality (m) is expressed as the amount of solute per 1 • Weight/volume solutions

kg of solvent.
• Molality Formula

• Volume/volume

Normality

• Normality (N) is the number of equivalent weights per 1

liter of solution • Weight/weight
• Normality Formula

Stoichiometry

Dimensional Analysis

• Dimensional analysis is a general problem-solving

Relationship between Molarity and Normality
method in which the units associated with numbers are
used as a guide in setting up calculations

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Steps to follow The Mole

Step 1: Identify the known or given quantity and the units of
the new quantity to be determined. Write an equation with the
given quantity on the left and the units of the desired quantity
on the right.
Step 2: Multiply the given quantity by one or more conversion
factors in such a manner that the unwanted (original) units are
canceled, leaving only the desired units
• The mole is the SI unit for the amount of substance
• It is defined as the amount of a substance that contains
the same number of entities as there are atoms in exactly
12g of carbon-12
• Constant (molecules/atoms)

Step 3: Perform the mathematical operations indicated by the

conversion factor setup.

Atomic Mass
Molar Mass
• The mass of atoms of elements expressed in atomic
• The molar mass is the mass, in grams, of a substance
mass units (amu)
that is numerically equal to the substance formula mass.
Molecular weight

• Sum of the atomic weights for the atoms in a molecule Chemical Formulas and the Mole concept
• For the molecule ethane, C2H6, the molecular weight
• Chemical formulas can be interpreted in two ways
would be
▪ For example, the formula N2O4

1st = The formula N2O4 contains two atoms of nitrogen and

four atoms of oxygen in one molecule of N2O4

2nd = The formula N2O4 contains 2 moles of nitrogen atoms

and 4 moles of oxygen atoms are present in one mole of N2O4

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The Mole and Chemical Calculations Conventions used in writing Chemical Equations

1. Reactants are always written on the left side of the

equation

2. Products are always written on the right side of the

equation

3. The reactants and the products are separated by an

arrow pointing towards the products

4. Plus, signs are used to separate different reactants or

different products

Balancing Chemical Equations

• A balanced chemical equation is a chemical equation

Writing and Balancing Chemical Equations
• A chemical equation is a written statement that uses
chemical symbols and chemical formulas to describe the
changes that occur in a chemical reaction
that has the same number of atoms of each element
involved in the reaction on each side of the equation
• An unbalanced chemical equation is brought into
balance by adding coefficients
• A coefficient is a number placed to the left of a
chemical formula in a chemical equation

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Chemical Equations and the Mole Concept • Analyte – a substance or sample being analyzed
• Bulk System – a term for the material under
• The coefficients in a balanced chemical equation can be
investigation (group)
interpreted in two ways
• Sample – representative portion of the bulk system
o The analytical laboratory technician analyzes
these samples by subjecting them to certain
rigorous laboratory operations that ultimately
1ST = One molecule of N2 reacts with three molecules of H2 to result in the identity or quantity of the analyte in
produce two molecules of NH3 question
▪ The key is that the sample must possess all
2ND= One mole of N2 reacts with three moles of H2 the characteristics of the entire bulk
to produce two moles of NH3 system with respect to the analyte and the
analyte concentration in the system
• The coefficients in a balanced chemical equation can be
▪ In other words, it must be a representative
used to generate mole-based conversion factors
sample – it must truly represent the bulk
system

REAGENTS AND SOLUTIONS CHEMICALS

• To learn about solutions, reagents, and different ANALYTICAL REAGENT (AR)

chemicals used in the clinical laboratory.
• Suitable for use in most analytic laboratory procedures
DEFINITION OF TERMS • The American Chemical Society established
specifications for AR grade chemicals
• REAGENT
• Labels on reagents state the actual impurities for each
▪ is a compound or mixture added to a system to
chemical lot or list the maximum allowable impurities
cause a chemical reaction
▪ It may be used to tell whether or not a specific
chemical substance is present by causing a
reaction to occur with it.

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ULTRAPURE o REAGENT GRADE WATER – CLRW/SRW

• Ultrapure chemicals have been put through additional Distilled Water

purification steps for use in specific procedures such as
• Distilled water has been purified to remove almost all
chromatography, atomic absorption, immunoassays,
organic materials, using distillation process in which
molecular diagnostics, standardization, or other
water is boiled and vaporized
techniques that require extremely pure chemicals.
Deionized Water
USP or NF
• Deionized water has some or all ions removed, usually
done from previously treated water, such as prefiltered
or distilled water

RO Water

• Chemicals that are used to manufacture drugs, may be
pure enough for use in most chemical procedures
CHEMICALLY PURE / PURE GRADE
• Reverse osmosis is a process that uses pressure to force
water through a semipermeable membrane, producing
water that reflects a filtered product of the original
water

• These designations indicate that the impurity limitations Ultrafiltered Water

are not stated and that preparation of these chemicals is
not uniform • Produced from the process of ultrafiltration, which
removes particulate matter, microorganisms, and any
pyrogens or endotoxins
TECHNICAL/COMMERCIAL GRADE

• WATER SPECIFICATIONS
o DISTILLED WATER
o DEIONIZED WATER
o RO WATER
o ULTRAFILTERED WATER

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Reagent grade water Solution

• Reagent grade water can be obtained by initially filtering • A solution is a homogenous mixture of two or more
it to remove particulate matter, followed by reverse substances with each substance retaining its own
osmosis, deionization, and a 0.2 mm filter or more chemical identity
restrictive filtration process.
Solvent
Type I Water
• A solvent is the component of solution that is present in
• Used for test methods requiring minimum interference, the greatest amount, the medium in which the other
such as trace metal, iron and enzyme analyses substances present are dissolved

Type II Water Solute

• Type II water is used for general laboratory applications • A solute is a component of a solution that is present in a
and is acceptable for most analytic requirements, lesser amount relative to that of the solvent.
including reagent, quality control and standard
Dilution
preparation
• Dilution is the process in which more solvent is added to
Type III Water
a solution in order to lower its concentration
• Type III water is acceptable for glassware washing and
Dilute Solution
filling autoclaves, but not for analysis or reagent
preparation • A dilute solution is one in which there is relatively little
solute or one which has been made to a lower solute
concentration per volume of solvent as when making a
SOLUTIONS
dilution.
• CONCENTRATION
Concentrated Solution
• COLLIGATIVE PROPERTIES
• A concentrated solution has a large quantity of solute in
solution

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Saturated Solution • Semi-analytical balance

o A lesser precision instrument than the analytical
• A saturated solution is a solution in which there is an
balance. The platform has no enclosures as the
excess of undissolved solute particles
readings usually only includes 1/10th of a gram.
Supersaturated Solution

• A supersaturated solution has an even greater

concentration of undissolved solute particles than a
saturated solution of the same substance

• Double beam balance

Instruments of Accuracy and Precision o A crude weighing tool that uses counterweights
to measure the weight of an analyte.
1. Balances

• Analytical Balance
o A weighing instrument with the platform
enclosed by glass doors in all directions. Sensitive
enough that a slight breeze could alter the 2. Caliper
reading.
• tool for precisely measuring length or diameter.
• 2 different sides can be used to measure inner and outer
diameter.

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3. Volumetric Glassware 5. Other tools for measurement

• Volumetric glasswares are used for precise and accurate • Mohr pipette
measurements as they are typically the instruments • Serological pipette
with the lowest margin of error.

• Graduated Cylinder

• Erlenmeyer Flask
Markings on Glasswares

4. Automatic Pipettes

• Pipettes with a built-in vacuum system that allows for • Beaker

consistent aspiration of a variable or fixed volume.
• Precision is high.
• Accuracy is only high if regularly maintained and
calibrated.

• Reagent Bottles

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Instruments of Separation 3. Pipettes should be washed regularly with mild detergent

and water. Take note that some chemicals can etch or
1. Centrifuge
damage glasswares, and thus alter the volume that it can
• Uses centrifugal force to separate suspended elements contain/transfer.
in a solution. 4. Instruments should not be used irresponsibly. There is
no <one-size-fits-all= for these instruments, and so, it is
important for you to find out if the instrument/glassware
can handle the experiment that you will be doing.

2. Filters PRECIPITATION METHOD

• Filters are used to remove suspended particles in a • PRECIPITATION REACTION

solution by the use of gravity (sometimes assisted by a ▪ Two Solutions are Mixed and an Insoluble
vacuum) Substance forms.
▪ Precipitate- This is insoluble Substance

• Is also known as ARGENTOMETRIC ANALYSIS- argentum-

silver

• Analyte is titrated with a standard solution of a

Instrument Care precipitating agent in the presence of an appropriate
indicator.
1. Like all other materials, it is important to read and
understand about the different requirements • It applies the solubility product principle, which states
to care for laboratory instruments. that in a saturated solution of an ionic compound, the
2. For machines, annual calibration is recommended. This product of the molar activities has a constant value at any
should be done by the manufacturer/distributor’s particular temperature and pressure.
authorized technicians.

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ENDPOINT COLORED ADSORPTION PRODUCT (FAJAN METHOD)

KAZIMIERS FAJAN
The endpoint is determined by
• Titrant/VS/Standard Solution = Silver Nitrate
- Formation of precipitate
• Indicator = DCF, TEE, Eosin Y
- Appearance of turbidity
• Endpoint = Yellowish green to reddish pink
- Instrumental methods
- Internal indicators
COMPOUNDS ASSAYED
INTERNAL INDICATORS
- Determination of Halogens
• COLORED ION – VOLHARD METHOD
- Thiocyanate
• COLORED PRECIPITATE – MOHR METHOD
- Cyanide
• COLORED ADSORPTION PRODUCT – FAJAN METHOD
STANDARD SOLUTIONS
COLORED ION (VOLHARD METHOD) JACOB VOLHARD • SILVER NITRATE - a colorless crystalline solid becoming
black on exposure to light. A silver salt with powerful
• Titrant/VS/Standard Solution = Ammonium thiocyanate
germicidal activity. It can potentially be used as
(NH4SCN)
cauterizing or sclerosing agent.
• Indicator = Ferric Alum or FAS (Ferric Ammonium Sulfate)
• AMMONIUM THIOCYANATE – a colorless crystalline
• Secondary precipitate = Ferric thiocyanate Fe (SCN)3
solid. It is soluble in water. It is used in chemical
• Endpoint = Reddish brown color
analysis, in photography, as a fertilize, and other uses.
COLORED SECONDARY PRECIPITATE (MOHR METHOD) KARL • POTASSIUM THIOCYANATE – an important salt of the
FRIEDRICH MOHR thiocyanate anion. The compound has a low melting
point relative to most inorganic salts.
• Titrant/VS/Standard Solution = Silver Nitrate
• Indicator = Potassium chromate (K2CrO4)
• Secondary precipitate = Silver chromate
• Endpoint = White to Reddish colored mixture

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DRYING AND IGNITING PRECIPITATES
PRECIPITATION
• Most precipitation gravimetric methods were developed
in the nineteenth century
• In precipitation gravimetry an insoluble compound
forms when we add a precipitating reagent, or
precipitant, to a solution that contains our analyte.
• In most cases the precipitate is the product of a simple
metathesis reaction between the analyte and the
precipitant; however, any reaction that generates a
precipitate potentially can serve as a gravimetric method.
• after the precipitate has been separated from the
solution, it has in some cases to be dried and then
weighed; in others, it has to be dried and ignited before
weighing
• The operations of drying and ignition and the necessary
apparatus will now be described.
DRYING AND IGNITING THE PRECIPITATE
• After separating the precipitate from its supernatant
solution, we dry the precipitate to remove residual traces
of rinse solution and to remove any volatile impurities.
• The temperature and method of drying depend on the
method of filtration and the precipitate’s desired
chemical form.
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• Placing the precipitate in a laboratory oven and heating
to a temperature of 110oC is sufficient to remove water
and other easily volatilized impurities.
• Higher temperatures require a muffle furnace, a Bunsen
burner, or a Meker burner, and are necessary if we need
to decompose the precipitate before its weight is
determined.
• A filter paper absorbs moisture, we must remove it
before we weigh the precipitate, this is accomplished by
folding the filter paper over the precipitate and
transferring both the filter paper and the precipitate to a
porcelain or platinum crucible.
• Fritted-glass crucibles cannot withstand high
temperatures and are dried in an oven at a temperature
below 200oC.
• The glass fiber mats used in Gooch crucibles can be
heated to a maximum temperature of approximately
500oC.
• Precipitates that are dried (below 250°C) or ignited
(above 250°C) should be collected on filter paper,
porcelain filtering crucibles or silica filtering crucibles.
The temperature at which precipitates are dried or
ignited can be determined by a study of
thermogravimetry.
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Thermogravimetry SOLUBLE SILVER SALTS SUCH AS SILVER(I)

• is a technique in which a change in the weight of a
substance is recorded as a function of temperature
or time. I
• t is used in conjunction with other techniques like
differential thermal analysis (DTA), gas
chromatography and mass spectrometry.
Crystalline precipitates
• absorb water or solvent can be easily removed by
heating the precipitates e. g. cuprous thiocyanate.
• NITRATE CAN BE USED AS PRECIPITATING AGENTS TO
DETERMINE THE AMOUNT OF HALIDE IONS PRESENT IN
A SAMPLE. NOT ONLY DOES THE MASS OF THE
PRECIPITATE TELL YOU ABOUT THE CONCENTRATION OF
THE HALIDE IONS IN SOLUTION, THE COLOR IS ALSO
DISTINCTIVE FOR DIFFERENT SILVER SALTS. THIS PICTURE
SHOWS TEST TUBES CONTAINING YELLOWISH AGI (LEFT),
CREAM-COLORED AGBR (MIDDLE), AND WHITE AGCL
(RIGHT)

CALCULATING RESULTS FROM GRAVIMETRIC DATA

APPLICATIONS OF GRAVIMETRIC METHODS

PRECIPITATION GRAVIMETRY DETERMINING THE PURITY OF A MIXTURE CONTAINING

• an analytical technique that uses a precipitation reaction
to separate ions from a solution
• The chemical that is added to cause the precipitation is
called the precipitant or precipitating agent.
• is a broader class of analytical techniques that includes
precipitation gravimetry and volatilization gravimetry.
MGCL2 AND NANO3
• As a result of the mishap, we have 0.7209 g of a
mysterious mixture containing MgCl2 and NaNO3. We
would like to know the relative amount of each
compound in our mixture, which is fully dissolved in
water. We add an excess of our precipitating agent
silver(I) nitrate, AgNO3(aq), and observe the formation of
a precipitate, AgCl(s). Once the precipitate is filtered and
dried, we find that the mass of the solid is 1.032 g.

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WHAT IS THE MASS PERCENT OF MGCL2 IN THE ORIGINAL STEP 1: CONVERT MASS OF PRECIPITATE, AGCL(S), TO
MIXTURE? MOLES

• Since this is a stoichiometry problem, we will want to
start with a balanced chemical equation. Here we are
interested in the precipitation reaction between
MgCl2(aq) and AgNO3(aq) to make AgCl(s), when
AgNO3(aq) is in excess.
• Since we are assuming that the mass of the precipitate is
all AgCl(s), we can use the molecular weight of AgCl to
convert the mass (grams) of precipitate to moles.

• You might remember that precipitation reactions are a

type of double replacement reaction, which means we STEP 2: CONVERT MOLES OF PRECIPITATE TO MOLES OF
can predict the products by swapping the anions (or MGCL2
cations) of the reactants. We might check our solubility
rules if necessary, and then balance the reaction. In this
problem we are already given the identity of the
precipitate, AgCl (s). That means we just have to identify • We can convert the moles of AgCl(s) , the precipitate, to
the other product,Mg(NO3)2 (aq), and make sure the moles of MgCl2(aq) using the molar ratio from the
overall reaction is balanced. The resulting balanced balanced equation
chemical equation is:

STEP 3: CONVERT MOLES OF MGCL2 TO MASS IN GRAMS

• Since we are interested in calculating the mass percent

• The balanced equation tells us that for every 1 mol MgCl2 of MgCl2 in the original mixture, we will need to convert
(aq), which is the compound we are interested in moles of MgCl2 into grams using the molecular weight
quantifying, we expect to make 2 mol AgCl(s), our
precipitate. We will use this molar ratio to convert moles
of AgCl(s) to moles of MgCl(2). We are also going to make
the following assumptions:

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STEP 4: CALCULATE MASS PERCENT OF MGCL2 IN THE MIXTURE

• The mass percent of MgCl2 in the original mixture can

be calculated using the ratio of the mass of MgCl2 from
Step 3 and the mass of the mixture

SHORTCUT: WE COULD ALSO COMBINE STEPS 1 THROUGH 3

INTO A SINGLE CALCULATION WHICH WILL INVOLVE CAREFUL
CHECKING OF UNITS TO MAKE SURE EVERYTHING CANCELS
OUT PROPERLY

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