LAS NO.

1: ANALYTICAL CHEMISTRY LABORATORY physicochemical properties of the components of a

mixture.
APPARATUS AND EQUIPMENT
Analytical Chemistry
LAS NO.3: IDENTIFICATION OF SELECTED IONS &
 a scientific discipline that develops and applies methods,
instruments, and strategies to gain information about the METALS
composition and nature of matter.  The identification of the various ions present in a
 An interdisciplinary branch of science that plays an sample is a common task in analytical chemistry.
important role in all streams of chemistry such as
inorganic, organic, physical, industrial, and biochemistry. Qualitative analysis
 Finds extensive applications in environmental science,  a common experimental method used to identify ions
agricultural science, oceanography, clinical chemistry, in a mixture.
solid-state research, and electronics.  The ions in a mixture are separated by selective
precipitation in qualitative analysis.
Laboratories  The addition of a properly selected reagent to an
 places where scientists and medical professionals aqueous mixture of ions results in the precipitation of
conduct studies to perform other work relevant fields. one or more of the ions while leaving the rest in
 contain equipment to help with experiments. solution.
 After isolating each ion, its identity can be confirmed
Laboratory apparatus and equipment using a chemical reaction particular to that ion.
 tools required to complete laboratory work.  Acid-base reactions, oxidation-reduction reactions,
 are used to measure, ignite, contain, hold, or weigh and the formation of complex ions are often used for
various substances for multiple purposes relating to the separating ions or for determining the presence of
experiment. specific ions.
 Classifications: (1) used to measure volume, (2) used to
measure weight, (3) used to measure length. Group IA Metals
 When making measurements, it is important to be as  Alkali metals: lithium, sodium, potassium, rubidium,
accurate and precise as possible. cesium, and francium
Examples:  The elements lie in the s-block as they have only one
o Volume: graduated cylinders, volumetric flasks, valence electron in their outer shell.
burettes, and pipettes.  They are ready to lose the valence electron to form a
o Weight: Analytical balances, top loading balances, and cation with charge +1 and achieve a stable octet
beam balances electronic configuration.
o Length: rulers, tape measures, micrometers, Vernier  Characteristics: malleable, ductile, good conductors of
caliper (most precise) heat and electricity, shiny, soft and can be cut easily
with a knife.
 Most laboratory apparatus are made of glass.  They never exist as free elements and are found
 Classification of glassware depending on their use; (1) naturally only in salts. They must be stored under oil
used to contain and (2) used to deliver. to prevent reaction with air due to high reactivity.
o Used to contain - apparatus that functions to contain  Group IA elements have similar physical and
samples as long as they can contain the sample. chemical characteristics.
o Used to deliver – apparatus that is used to measure
and deliver specific amounts of sample. It has the Group IIA Metals
characteristic of delivering accurate and precise  Elements include Be, Mg, Ca, Sr, Ba and Ra are all
amounts of samples. metals, but only Be and Mg are active metals.
 Often called alkaline-earth metals. The term
alkaline reflects the fact that many compounds of
LAS NO.2: ANALYTICAL LABORATORY TECHNIQUES AND
these metals are basic or alkaline. The term earth was
OPERATIONS used to describe that many of these compounds are
Laboratory work insoluble in water.
 requires the use of tools that enable the efficient  Most of the chemistry of the alkaline-earth metals
execution of basic techniques. (Group IIA) can be predicted from the behavior of the
alkali metals (Group IA).
Basic laboratory operations  Alkaline-earth metals tend to lose two electrons to
 are grouped methods and general procedures that enable form M 2+ ions (Be2+, Mg2+, Ca2+, and so on). These
a successful analytical experiment to be performed. metals are less reactive than the neighboring alkali
 When a procedure is carried out, protocol begins with the metal.
choice of chemicals, reagents, and solvents that must be
measured. It continues with the reaction, for which the Group IB Metals
solid or liquid reagents must be transferred, mixed,  Metals Copper, Silver, and Gold, are known as
stirred, heated, or cooled for certain periods and at coinage/noble or Group 11 metals.
certain temperatures. This will require specific  Classified as d-block or transition metals.
operations depending on the nature and properties of  They are relatively inert and corrosion-resistant
these products depending on the different 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

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
The requirements for titrimetric analysis are the maybe standardized using standard solutions of
following: hydrochloric acid or sulfuric acid as a secondary standard,
1. Reaction must be complete. or potassium biphthalate as a primary standard. Thus, the
2. Must have an end point detecting device. solution will be conducted in a direct acidimetric
3. Must be rapid. neutralization analysis.
4. Must have a sharp endpoint.
Differentiate primary standard from secondary standard. SPECTROCHEMICAL ANALYSIS
Secondary standard is another standard solution used to  are techniques for chemical analysis that rely on the
determine the concentration of another solution whereas measurement of electromagnetic radiation's
primary standard is a carefully weighed sample of a substance wavelength and intensity. On the basis of the amounts
of known purity. of energy absorbed during changes in the structure or
Indicate the chemical reaction involved in the motion of the molecules, it is mostly used to
standardization of 1 N sodium hydroxide solution. determine the arrangement of atoms and electrons in
KHC8H4O4 + NaOH → KNaC8H4O4 + H2O molecules of chemical compounds.
How would the standard solution of sulfuric acid be
stored? Activity Questions:
Sulfuric acid should be stored in a cool, dry area away from What is the purpose of warming-up the instrument?
direct sunlight, heat, and ignition sources, and that is separate By warming up an instrument you insure that all the
from incompatible materials. Standard solutions of sulfuric components have reached a uniform operating
acid are preserved in a tightly stoppered, alkali-free bottles to temperature. It will also drive off any moisture that may
prevent deterioration. have condensed inside the unit. The spectrometer should
be allowed to warm up for at least fifteen minutes to
What is the other method of standardizing sulfuric acid stabilize the source and detector
solution?
It can also be standardized gravimetrically by precipitation What is the use of a cuvette? Why is not an ordinary
and weighing an equivalent amount of barium sulfate, as test tube/vial used?
described under the gravimetric determination of sulfate in a The cuvette is rectangular test tubes. They are used to
soluble sulfate. hold aqueous solutions like normal test tubes. Normal test
tubes are useful in chemical reactions. In contrast,
Give the chemical reaction involved in the standardization cuvettes are used in UV-Vis spectrophotometer or
of 1 N sulfuric acid. fluorometer for the measurement of transmittance or
NaOH + H2SO4 → Na2SO4 + H2O absorbance of radiation at a particular wavelength. The
key difference between cuvette and test tube is that the
LAS 8: ASSAY OF MILK OF MAGNESIA / MAALOX cuvette has two straight sides whereas the test tube has no
Activity Questions: straight sides. Further, cuvettes and test tubes have
What type of titration is involved in the assay of milk of different applications and chemical compositions as well.
magnesia or Maalox?
Assay of magnesium hydroxide follows acid-base reaction in
which a standard acid is used. Mg(OH)2 is practically insoluble What is a blank solution? What is its role in
in water, direct titration is not possible. Thus, back or residual spectrochemical analysis?
titration is employed. The Mg(OH)2 content of MOM or Maalox A solution that does not contain a detectable amount of the
is assayed under the residual acidimetric neutralization analyte of interest. The blank solution is typically used for
analysis. calibration purposes. This ensures the absorbance
measured in the samples is attributed only to the sample
What are the standard solutions used in the assay? material and not the components of the solution the
Explain why they are used. sample is suspended in or the cuvette.
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 What is the relationship between absorbance and
H2SO4 solution to ensure complete neutralization of all the concentration?
Mg(OH)2 w/ the formation of the soluble magnesium sulfate. As the concentration goes up, more radiation is absorbed
The excess acid is then determined by residual titration with 1 and the absorbance goes up. Therefore, the absorbance is
N NaOH solution, using methyl red as an indicator. directly proportional to the concentration.

Write the chemical reactions involved when the Milk of Absorbance

Magnesia or Maalox is dissolved and upon residual  Beer-Lambert Law (Beer’s Law) - the linear
titration. relationship between absorbance and concentration
H2SO4 + Mg(OH)2 → 2 H2O + MgSO4 of an absorbing species.
MgSO4 + 2 NaOH → Mg(OH)2 + Na2SO4
Formula: A=abc
where: “A” - absorbance
“a” - molar absorptivity in L/[(mole)(cm)]
LAS 9: SPECTROCHEMICAL ANALYSIS – THE
“b” - path length in cm
UV/VISIBLE SPECTROPHOTOMETER “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 %.