LAS NO.
1: ANALYTICAL CHEMISTRY LABORATORY physicochemical properties of the components of a
APPARATUS AND EQUIPMENT
Analytical Chemistry
 a scientific discipline that develops and applies methods,
instruments, and strategies to gain information about the
composition and nature of matter.
 An interdisciplinary branch of science that plays an
important role in all streams of chemistry such as
inorganic, organic, physical, industrial, and biochemistry.
 Finds extensive applications in environmental science,
agricultural science, oceanography, clinical chemistry,
solid-state research, and electronics.
Laboratories
 places where scientists and medical professionals
conduct studies to perform other work relevant fields.
 contain equipment to help with experiments.
Laboratory apparatus and equipment
 tools required to complete laboratory work.
 are used to measure, ignite, contain, hold, or weigh
various substances for multiple purposes relating to the
experiment.
 Classifications: (1) used to measure volume, (2) used to
measure weight, (3) used to measure length.
 When making measurements, it is important to be as
accurate and precise as possible.
Examples:
o Volume: graduated cylinders, volumetric flasks,
burettes, and pipettes.
o Weight: Analytical balances, top loading balances, and
beam balances
o Length: rulers, tape measures, micrometers, Vernier
caliper (most precise)
 Most laboratory apparatus are made of glass.
 Classification of glassware depending on their use; (1)
used to contain and (2) used to deliver.
o Used to contain - apparatus that functions to contain
samples as long as they can contain the sample.
o Used to deliver – apparatus that is used to measure
and deliver specific amounts of sample. It has the
characteristic of delivering accurate and precise
amounts of samples.
LAS NO.2: ANALYTICAL LABORATORY TECHNIQUES AND
OPERATIONS
Laboratory work
 requires the use of tools that enable the efficient
execution of basic techniques.
Basic laboratory operations
 are grouped methods and general procedures that enable
a successful analytical experiment to be performed.
 When a procedure is carried out, protocol begins with the
choice of chemicals, reagents, and solvents that must be
measured. It continues with the reaction, for which the
solid or liquid reagents must be transferred, mixed,
stirred, heated, or cooled for certain periods and at
certain temperatures. This will require specific
operations depending on the nature and properties of
these products depending on the different
mixture.
LAS NO.3: IDENTIFICATION OF SELECTED IONS &
METALS
 The identification of the various ions present in a
sample is a common task in analytical chemistry.
Qualitative analysis
 a common experimental method used to identify ions
in a mixture.
 The ions in a mixture are separated by selective
precipitation in qualitative analysis.
 The addition of a properly selected reagent to an
aqueous mixture of ions results in the precipitation of
one or more of the ions while leaving the rest in
solution.
 After isolating each ion, its identity can be confirmed
using a chemical reaction particular to that ion.
 Acid-base reactions, oxidation-reduction reactions,
and the formation of complex ions are often used for
separating ions or for determining the presence of
specific ions.
Group IA Metals
 Alkali metals: lithium, sodium, potassium, rubidium,
cesium, and francium
 The elements lie in the s-block as they have only one
valence electron in their outer shell.
 They are ready to lose the valence electron to form a
cation with charge +1 and achieve a stable octet
electronic configuration.
 Characteristics: malleable, ductile, good conductors of
heat and electricity, shiny, soft and can be cut easily
with a knife.
 They never exist as free elements and are found
naturally only in salts. They must be stored under oil
to prevent reaction with air due to high reactivity.
 Group IA elements have similar physical and
chemical characteristics.
Group IIA Metals
 Elements include Be, Mg, Ca, Sr, Ba and Ra are all
metals, but only Be and Mg are active metals.
 Often called alkaline-earth metals. The term
alkaline reflects the fact that many compounds of
these metals are basic or alkaline. The term earth was
used to describe that many of these compounds are
insoluble in water.
 Most of the chemistry of the alkaline-earth metals
(Group IIA) can be predicted from the behavior of the
alkali metals (Group IA).
 Alkaline-earth metals tend to lose two electrons to
form M 2+ ions (Be2+, Mg2+, Ca2+, and so on). These
metals are less reactive than the neighboring alkali
metal.
Group IB Metals
 Metals Copper, Silver, and Gold, are known as
coinage/noble or Group 11 metals.
 Classified as d-block or transition metals.
 They are relatively inert and corrosion-resistant
metals, making them suitable for coin production.
  All three metals are excellent electrical and thermal
conductors. Identification Tests for Group IB, IIIB and Trace
 Silver is the most electrically conductive metal, followed Metals
by Copper and then Gold. REAGENT ION/METAL RESULT
 Silver is the most thermally conductive and light- Ammonium Azure blue
Copper (Cu2+)
reflective element. hydroxide solution
 They are ineffective as weapons or tools because they are Zinc White precipitate
all soft metals. Colorless
Cadmium
 Used to make ornaments and jewelry due to their solution
malleability. White gelatinous
Aluminum
solution
Group IIB Metals Bluish-green
Nickel
 Zinc Group/Group 12/IIB: zinc (Zn), cadmium (Cd), solution
mercury (Hg), and copernicium (Cn). Cobalt Pink solution
 Zinc, cadmium, and mercury are metals with a silvery- Iron (Fe3+ Reddish brown
white appearance and relatively low melting points and Brick red or red
Potassium
boiling points Copper (Cu2+) brown
ferrocyanide
 Mercury is the only metal that is liquid at room precipitate
temperature, and its boiling point is lower than that of Zinc White precipitate
any other metal. White flocculent
Cadmium
 The metals are significantly more electropositive than the precipitate
group 11 elements, so they are less noble. Prussian blue
Iron (Fe3+)
 The group 12 elements, whose chemistry is dominated by precipitate
the +2 oxidation state, are almost always found in nature Ferrous ion pale green
Acetic acid
combined with sulfur. (Fe2+) solution
Ferric ion (Fe3+) deep red solution
Trace Elements/Ions Sodium fluoride +
 Minerals known as trace elements or trace metals are Alcoholic
Cobalt blue-green color
minute levels which are found in living tissues. ammonium
 Commonly found trace elements are iron, zinc, fluoride, thiocyanate
selenium, copper, chromium, iodine, manganese, and Hydrochloric acid + Blue color which
Chromium
molybdenum. Hydrogen peroxide fades rapidly
 Trace elements function primarily as catalysts in enzyme
systems; some metallic ions, such as iron and copper, LAS NO.4: ANALYSIS OF GROUPS I and II CATIONS
participate in oxidation-reduction reactions in energy
 Metallic element analysis in compounds or samples is
metabolism.
an essential part of chemical research.
 The systematic analysis of cations is an essential
Identification Tests for Groups IA and IIA Metals
component of salt analysis (or systematic qualitative
REAGENT ION/METAL RESULT
analysis).
PRESENT
 Group I cations are those that selectively precipitate
pale yellow or
Magnesium uranyl as chlorides when diluted hydrochloric acid is added.
Sodium lemon yellow
acetate These cations are: Ag+ , Pb2+, and Hg2 2+.
solution
 The only elements whose chlorides are insoluble are
Lead (II) nitrate Sodium white precipitate
silver, lead (II), and mercury (I). These metals are less
Lead (II) nitrate Potassium yellow precipitate
reactive than their alkali metal neighbors.
white crystalline
Tartaric acid Potassium  In 0.1 to 0.3 M hydrochloric acid solution, group II
precipitate
cations react with H2S to form insoluble sulfides such
Sodium carbonate Lithium white precipitate
as HgS, PbS, Bi2S3, CuS, CdS, As2S3, SnS2, and Sb2S3.
Sulfuric acid Lithium white precipitate
 The copper subgroup includes the first five cations
Acetic acid + oxalic white octahedral
Calcium (Hg2+, Pb2+, Bi3+, Cu2+, Cd2+). Because their
acid precipitate
sulfides are not acidic, they are not soluble in KOH
Potassium oxalate Magnesium white precipitate,
solution.
Potassium chromate Barium yellow precipitate
 The last three cations (As3+, Sn4+, Sb3+) are arsenic
subgroup cations that form acidic sulfides that are
FLAME TEST
soluble in KOH and thus separable from the copper
ION/METAL PRESENT COLOR OF THE FLAME subgroup.
Sodium (Na) Golden yellow
Potassium (K) Violet/Purple
Lithium (Li) Carmine red
Calcium (Ca) Brick Red
Magnesium (Mg) Colorless
Barium (Ba) Apple Green
 Analysis of Group I Cations Neutralization Reaction
REAGENT ION/METAL RESULT  a chemical process in which an acid (proton donor)
PRESENT reacts with a base (proton acceptor). The products of
6M acetic acid + 1M Ag+ ion brick red neutralization reaction in aqueous solutions are salt
potassium chromate precipitate and water.
Sodium carbonate Pb2+ ion white precipitate
6M HCl Ag+ ion white curdy Standardizing a solution
precipitate  refers to the process of determining an unknown
Ammonium Ag+ ion metallic silver color concentration of substance within a solution.
hydroxide + Formic
acid Standard Solution
Ammonium Hg2 2+ ion gray to black  a solution of accurately known concentration
hydroxide precipitate prepared from a primary standard (a compound
which is stable, of high purity, highly soluble in water
Analysis of Group II Cations and of a high molar mass to allow for accurate
REAGENT ION/METAL RESULT weighing) that is weighed accurately and made up to
PRESENT a fixed volume.
Stannous chloride Mercuric (Hg2+) white or gray Indicator
solution ion precipitate  a chemical which changes color at or very near the
point in the titration where equivalent quantities of
Conc. Ammonium
analyte and titrant have reached.
hydroxide + water + Bismuth (Bi3+) immediate
potassium stannite ion blackening
solution LAS 6: ASSAY OF SODIUM BICARBONATE
Conc. Nitric acid + Definition of terms:
Arsenic (As3+) reddish brown
silver nitrate + a. Titration - The act of adding and measuring the
ion precipitate
sodium acetate volume of titrant used in the assay.
Arsenic (As3+)
Tin + 1-peso coin Black deposits
ion b. Analyte - It is the chemical substance or the active
Sodium nitrite + Antimony constituent in the sample being analyzed in the
lavender shade titration. It is also known as titrand.
conc. HCl (Sb3+) ion
3N HCl + Mg ribbon white or gray
Tin (Sn+4) ion c. Titrant - It is the solution of known concentration. It
+ Mercuric chloride precipitate
may also be called as the titrator, the reagent, or the
d. standard solution used in titration.
LAS 5: PREPARATION AND STANDARDIZATION OF
e. Indicator - It is usually a chemical which changes
0.1 N SULFURIC ACID color at or very near the point in the titration where
VOLUMETRIC ANALYSIS equivalent quantities of analyte and titrant have
 determination of the volume of a solution of known reacted.
concentration required to react with a given substance to
be analyzed. It is an analytical method in which the f. Stoichiometric point - point of a chemical reaction
volume of known concentration consumed during the at which chemically equivalent quantities of reactants
analysis is taken as a measure of the amount of active have been mixed. It is the theoretical point at which
constituent om a sample being analyzed. The type of equivalent amounts of each have reacted or also
titration in volumetric analysis are direct titration, known as equivalence point.
residual or back titration and blank titration.
g. End point - The point at which the reaction seems to
be completed. It comes after the stoichiometric point
which can be observed practically.

LAS 7: PREPARATION AND STANDARDIZATION

The requirements for titrimetric analysis are the
following:
1. Reaction must be complete.
2. Must have an end point detecting device.
3. Must be rapid.
4. Must have a sharp endpoint.
OF 1N SODIUM HYDROXIDE AND 1N SULFURIC
ACID SOLUTIONS
Activity Questions:
How will an alkali solution like sodium hydroxide be
standardized?
Solutions of sodium hydroxide in any concentration
maybe standardized using standard solutions of
hydrochloric acid or sulfuric acid as a secondary standard,
or potassium biphthalate as a primary standard. Thus, the
solution will be conducted in a direct acidimetric
neutralization analysis.
Differentiate primary standard from secondary standard.
Secondary standard is another standard solution used to
determine the concentration of another solution whereas
primary standard is a carefully weighed sample of a substance
of known purity.
Indicate the chemical reaction involved in the
standardization of 1 N sodium hydroxide solution.
KHC8H4O4 + NaOH → KNaC8H4O4 + H2O
How would the standard solution of sulfuric acid be
stored?
Sulfuric acid should be stored in a cool, dry area away from
direct sunlight, heat, and ignition sources, and that is separate
from incompatible materials. Standard solutions of sulfuric
acid are preserved in a tightly stoppered, alkali-free bottles to
prevent deterioration.
What is the other method of standardizing sulfuric acid
solution?
It can also be standardized gravimetrically by precipitation
and weighing an equivalent amount of barium sulfate, as
described under the gravimetric determination of sulfate in a
soluble sulfate.
Give the chemical reaction involved in the standardization
of 1 N sulfuric acid.
NaOH + H2SO4 → Na2SO4 + H2O
LAS 8: ASSAY OF MILK OF MAGNESIA / MAALOX
Activity Questions:
What type of titration is involved in the assay of milk of
magnesia or Maalox?
Assay of magnesium hydroxide follows acid-base reaction in
which a standard acid is used. Mg(OH)2 is practically insoluble
in water, direct titration is not possible. Thus, back or residual
titration is employed. The Mg(OH)2 content of MOM or Maalox
is assayed under the residual acidimetric neutralization
analysis.
What are the standard solutions used in the assay?
Explain why they are used.
1 N Sulfuric acid and 1 N NaOH solutions were used in the
assay. It is dissolved in an accurately measured excess of 1 N
H2SO4 solution to ensure complete neutralization of all the
Mg(OH)2 w/ the formation of the soluble magnesium sulfate.
The excess acid is then determined by residual titration with 1
N NaOH solution, using methyl red as an indicator.
Write the chemical reactions involved when the Milk of
Magnesia or Maalox is dissolved and upon residual
titration.
H2SO4 + Mg(OH)2 → 2 H2O + MgSO4
MgSO4 + 2 NaOH → Mg(OH)2 + Na2SO4
LAS 9: SPECTROCHEMICAL ANALYSIS – THE
UV/VISIBLE SPECTROPHOTOMETER
SPECTROCHEMICAL ANALYSIS
 are techniques for chemical analysis that rely on the
measurement of electromagnetic radiation's
wavelength and intensity. On the basis of the amounts
of energy absorbed during changes in the structure or
motion of the molecules, it is mostly used to
determine the arrangement of atoms and electrons in
molecules of chemical compounds.
Activity Questions:
What is the purpose of warming-up the instrument?
By warming up an instrument you insure that all the
components have reached a uniform operating
temperature. It will also drive off any moisture that may
have condensed inside the unit. The spectrometer should
be allowed to warm up for at least fifteen minutes to
stabilize the source and detector
What is the use of a cuvette? Why is not an ordinary
test tube/vial used?
The cuvette is rectangular test tubes. They are used to
hold aqueous solutions like normal test tubes. Normal test
tubes are useful in chemical reactions. In contrast,
cuvettes are used in UV-Vis spectrophotometer or
fluorometer for the measurement of transmittance or
absorbance of radiation at a particular wavelength. The
key difference between cuvette and test tube is that the
cuvette has two straight sides whereas the test tube has no
straight sides. Further, cuvettes and test tubes have
different applications and chemical compositions as well.
What is a blank solution? What is its role in
spectrochemical analysis?
A solution that does not contain a detectable amount of the
analyte of interest. The blank solution is typically used for
calibration purposes. This ensures the absorbance
measured in the samples is attributed only to the sample
material and not the components of the solution the
sample is suspended in or the cuvette.
What is the relationship between absorbance and
concentration?
As the concentration goes up, more radiation is absorbed
and the absorbance goes up. Therefore, the absorbance is
directly proportional to the concentration.
Absorbance
 Beer-Lambert Law (Beer’s Law) - the linear
relationship between absorbance and concentration
of an absorbing species.
Formula: A=abc
where: “A” - absorbance
“a” - molar absorptivity in L/[(mole)(cm)]
“b” - path length in cm
“c” - concentration of analyte (sample) in mol/L
LAS 10: THIN LAYER CHROMATOGRAPHY
CHROMATOGRAPHY
 a technique used for the analysis and separation of
chemical mixtures. The technique is based on a
polarity interplay between the sample and two other
substances called the solid or stationary phase and
 the mobile phase or eluent, which can be a liquid or a gas. PROBLEM SOLVING:
1. Calculate the normality of the solution of sulfuric acid if 26.4ml of
As their names indicate, the stationary phase does not
the solution reacts completely with 0.14g of sodium carbonate.
move, whereas the mobile phase flows across, or through
the solid phase.
 sample to be separated first becomes adsorbed onto the
surface of the solid phase through polar interactions.
More polar samples adhere (or bind) more strongly than
less polar ones. The mobile phase then comes in and
sweeps across the stationary phase, competing for the
sample. If the mobile phase is a solvent, it is called the
2. Find the purity percentage of 7.5g H2SO4 neutralized completely
eluting solvent. The more polar the solvent, the greater by 80 ml of 1.32N NaOH solution.
its capacity to carry the components of the mixture with
it, “yanking” them away from the solid phase as it moves.
Different components with different polarities will travel
at different rates as the solvent moves, causing their
separation.
 The most used solid adsorbents as stationary phases in
laboratory are silica gel and alumina due to their versatile
polarity range. In Thin Layer Chromatography, the solid
phase (silica gel or alumina) is applied as a thin coating 3. If a 0.2800 g sample of Sodium bicarbonate (96.5%) is titrated with
on a plastic sheet or glass slide, called a TLC plate. Using a 0.9231N Sulfuric acid, what volume of the acid should be required
to reach the end point?
capillary tube, spot applicator or toothpick, a solution of
the sample is applied on the solid support as a spot, a
technique known as spotting. When the sample dries it
becomes adsorbed onto the solid support. This process
can be repeated several times to produce a more
concentrated spot.

TYPES OF CHROMATOGRAPHY
4. If 25.00 mL of a sodium hydroxide solution required 40.00 mL of a
MOBILE PHASE STATIONARY sulfuric acid solution in a titration and 25.00 mL of the sulfuric acid
PHASE solution was required in the titration of 0.3060 g of pure sodium
LIQUID LIQUID SOLID BEADS carbonate, what was the Normality of the sodium hydroxide
solution?
CHROMATOGRAPHY
GAS GAS LIQUID/SOLID
CHROMATOGRAPHY
PAPER LIQUID PAPER STRIP
CHROMATOGRAPHY
THIN-LAYER LIQUID Plate covered
CHROMATOGRAPHY with a thin layer
of alumina or
silica gel 5. If 18.50 mL of 0.1173 N sodium hydroxide and 20 mL of sulfuric
acid were utilized to reach the endpoint of titration, calculate the
FORMULAS: Normality of the acid.

6. What is the volume of the standard base solution (0.9520 N) if it

consumed an exactly 25.00 mL of 0.9781 N sulfuric acid during
titration?
7. Calculate the Mg(OH)2 content of Milk of Magnesia, 12.32 g of which 13. If a 0.3753 g sample of sodium bicarbonate (80.9%) is titrated
was dissolved in 50 mL of 1.0340 N sulfuric acid producing a mixture with 0.9155N sulfuric acid, What volume of the acid should be
that required 24.6 mL of 1.1255 N sodium hydroxide. required to produce an end point?

8. Express the following absorbance values in percentage transmittance: 14. Calculate the Sodium carbonate content of 1.12g sample requiring
a. 0.0356 24.8ml of 0.1947N HCL on titration with phenolphthalein
b. 0.379
c. 0.485

9. Convert the following percentage transmittance values to absorbance:

a. 27.2% =
b. 30.6% =
c. 0.093% =

10. A solution of serum albumin was analyzed using spectrophotometric

analysis and yielded an absorbance (ABS) reading of 0.3531. The
cuvette is measured to have a length of 5 cm and the molar absorptivity 15. Calculate the Mg(OH)2 content of milk of magnesia, 3.53g of which
coefficient of serum albumin is 43,824M-1 cm-1. Compute for the was dissolved in 50.00ml of 1.0340N Sulfuric acid, producing a
concentration of serum albumin. mixture that required 18.20ml of 1.1255ml N Sodium Hydroxide

11. Compute for the concentration of an alcoholic solution of methylene

blue with an absorbance (ABS) reading of 0.6583. A standard 16. If a 1.54g sample of zinc oxide, 96.2%, were treated with 50ml of
calibration was done which yielded the following result: 1.0923N H2SO4 in the usual way, what volume of 0.9765N sodium
Hydroxide would be required in the back titration?

17. A 4.0520g sample of HCl, sp. Gr 11.18, required 44.15ml of

0.9035M of Sodium Hydroxide in titration, compute for percent
purity.

12. A solution of Potassium permanganate with a concentration of 7.30 x 10

-5 M yields a transmittance of 24.4% when measured in a 5-cm cell
compartment at a wavelength of 525 nm. Calculate:
a. Absorbance of the solution

b. Molar absorptivity coefficient of KMnO4

18. A Sodium Chloride (0.1920g) NaCl was assayed using volhard
Method, using 52mL of 0.0975N AgNO3 and 12.3 mL of
0.1192Ammonium thioscyanate. Calculate the sample in %.