CHE029

MODULE 6-10 – Analytical Chemistry CHEMICAL REACTION OF SODIUM BICARBONATE W/

Lesson title: Laboratory Lessons O.1 N SULFURIC ACID
NaHCO3 + H2SO4 → Na2SO4 + 2CO2 + 2H2O
Coverage: - In this reaction, sodium bicarbonate (NaHCO3) acts as
• Assay of Sodium Bicarbonate a base and sulfuric acid (H2SO4) acts as an acid. When
• Sodium Hydroxide the two are mixed together, the acid and base
• Assay of Milk of Magnesia (MAALOX) neutralize each other, forming Sodium sulfate
• Spectrochemical Analysis (Na2SO4), carbon dioxide (CO2), and water (H2O)
• Thin Layer Chromatography
PREPARATION AND STANDARDIZATION OF 1N SODIUM
INTRODUCTION HYDROXIDE AND 1N SULFURIC ACID
VOLUMETRIC ANALYSIS - Solutions of Sodium hydroxide in any concentration
- The determination of the volume of a solution of maybe standardized using standard solutions of
known concentration required to react with a given hydrochloric acid or sulfuric acid as a secondary
substance to be analyzed standard, or potassium biphthalate as a primary
It needs the following components so that the assay can standard
proceed: - Thus, the solution will be conducted in a direct
1. Analyte – the substance to be assayed acidimetric neutralization analysis
2. Titrant – the substance of known concentration - Carbon-dioxide free water is used in order to avoid
3. Indicator – an organic compound that changes color to chemical reactions that leads to formation of
signal that a chemical reaction has occurred carbonates and to accurately compute for the
ASSSAY OF SODIUM BICARBONATE (Na2HCO3) normality of a substance
Procedure: - The solution can be treated also with barium
1. Ask your instructor for the sodium bicarbonate powder hydroxide to precipitate any carbonate formed
(sample) and the total weight of the sample through the action of carbon dioxide on the Sodium
to be analyzed. Hydroxide
2. Transfer the sodium bicarbonate powder into the 250- - The sodium hydroxide solution is preserved in a
mL Erlenmeyer flask. tightly stoppered bottle fitted with a soda-lime tube
3. Using a graduated cylinder, measure 25 mL of distilled to protect it from the carbon dioxide of the air
water. Transfer the distilled water into the - Solutions which contain carbonates are not suitable
Erlenmeyer flask that contains the powder. for titration if phenolphthalein indicator is used but
4. Add two drops of Methyl red T.S. into the flask that Methyl orange can be used in the titration which will
contains the sodium bicarbonate solution. provide the same results as long as all the sodium
5. Titrate it with the 0.1 N of Sulfuric acid (from Activity present were combined as hydroxides
No.5), until endpoint is reached. Using an acid - Sulfuric acid solutions are preferable in hot titrations
burette (mount the acid burette in an/a iron stand or ring since there would be a risk of losing the acid due to
stand by means of a burette clamp), slowly volatilization
add the 0.1 N Sulfuric acid with constant stirring until the - Standard solutions of sulfuric acid are preserved in a
solution in the Erlenmeyer flask becomes tightly stoppered, alkali-free bottles to prevent
faintly pink. deterioration
6. Heat the solution (if necessary) and continue the I. PREPARATION
titration. Procedure:
7. Heat again and titrate further as necessary until the pink 1. Prepare a carbon-dioxide free water. This will be
color becomes permanent. prepared by boiling a 500 mL of distilled
8. Measure the volume (mL) of sulfuric acid used to reach water in a beaker for 5 min while covered in a watch glass.
the end point Allow the water to stand and cool
at room temperature. Note: Do not allow the water to be
exposed in the air to prevent CO2 absorption
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2. Measure 100 mL of carbon-dioxide free water using a PREPARATION AND STANDARDIZATION OF 1 N

graduated cylinder. Transfer SULFURIC ACID SOLUTION
immediately the measured carbon-dioxide free water into I. PREPARATION
150-mL beaker and cover it with a Procedure:
watch glass. 1. Place about 200 mL of distilled water in a 250-mL
3. Weigh 11.25 g of sodium hydroxide pellets. Carefully volumetric flask.
dissolve the weighed NaOH pellets 2. Using a graduated pipette and aspirator pump, add 7.5
into the beaker containing the carbon-dioxide free water. mL of concentrated sulfuric acid
4. Allow the solution to stand and cool at room slowly in the distilled water while stirring continuously.
temperature. Filter the solution (perform 3. Add enough distilled water to make 250 mL of final
filtration set-up and process) and use another 150-mL volume.
beaker as a receiving container. 4. Allow the solution to stand and cool at room
5. Transfer the filtered solution in a 250-mL volumetric temperature.
flask then add enough distilled water to
make 250 mL of final volume. II. STANDARDIZATION
Procedure:
II. STANDARDIZATION (NaOH) 1. Transfer 20 mL of sulfuric acid solution from B.I.
Procedure: (Preparation) into the 250-mL Erlenmeyer
1. Weigh accurately about 5 g of Potassium Hydrogen flask. Add 2 drops of phenolphthalein T.S.
phthalate (biphthalate) that has been 2. Using a burette (mount the burette in an/a iron stand
previously crushed and heated in the laboratory oven or or ring stand by means of a burette
incubator at a temperature of 120°C clamp), slowly add the previously standardized sodium
for 2 hours. hydroxide from Experiment A until a
2. Using a 100-mL graduated cylinder, measure 75 mL of permanent light pink color is obtained while swirling
carbon-dioxide free water and constantly under heating.
transfer this into the 250-mL Erlenmeyer flask. FORMULA:
3. Dissolve the 5 g of crushed and heated potassium Vacid x Nacid = Vbase x Nbase
hydrogen phthalate (biphthalate) into the 𝑉 𝑁𝑎𝑂𝐻 𝑥 𝑁 𝑁𝑎𝑂𝐻
N= H2SO4 = 𝑉 𝐻2𝑆04
Erlenmeyer flask containing the carbon-dioxide free
water. Add 2 drops of Phenolphthalein
CHEMICAL REACTION 1 N SODIUM HYDROXIDE
T.S.
4. Using a burette (mount the burette in an/a iron stand SOLUTION
or ring stand by means of a burette NaOH + KHC8H4O4 → KNaC8H4O4 + H2O
clamp), slowly add the prepared base (sodium hydroxide - In this reaction, Sodium Hydroxide reacts with
solution) from Experiment A.I. potassium hydrogen phthalate to form
(Preparation) with constant stirring until the solution in Potassium Sodium Phthalate and water
the Erlenmeyer flask produces a
permanent pink color. ASSAY OF MILK OF MAGNESIA / MAALOX
5. Measure the volume (mL) of sodium hydroxide solution MAGNESIUM HYDROXIDE
used.
- As an antacid preparation is commonly known as
“Milk of Magnesia” (MOM)
FORMULA:
𝑤𝑡. 𝑜𝑓 𝑝𝑟𝑖𝑚𝑎𝑟𝑦 𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝐾𝐻𝐶8𝐻404
- MOM is an antacid suspension that neutralizes
𝑁= acid in the stomach. The side effect of which is
𝑣𝑜𝑙 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑥 𝑚𝐸𝑞 𝑤𝑡. 𝑜𝑓 𝐾𝐻𝐶8𝐻404
Diarrhea
- It is usually available in the market in
combination with Aluminum hydroxide to
Neutralize Magnesium hydroxide’s side effect.
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- The common brand name and available UV-Vis SPECTROSCOPY

suspension product in combination is Maalox® - Is an analytical technique that compares the
- Assayed under the residual acidimetric amount of discrete wavelengths of UV or visible
neutralization analysis since solutions of sulfuric light absorbed or transmitted by a sample to a
acid and sodium hydroxide are used. reference or blank sample
- It is dissolved in an accurately measured excess - Widely used technique in many fields of science,
of 1 N Sulfuric acid solution to ensure complete including Bacterial culture, drug identification,
neutralization of all the Magnesium hydroxide and Nucleic acid Purity checks and
with the formation of the soluble Magnesium quantification, as well as quality control in the
sulfate. beverage industry and chemical research
- The excess acid is then determined by residual
titration with 1 N sodium hydroxide solution,
using Methyl red as an indicator

% 𝑀𝑔(𝑂𝐻)2
[(𝑉𝐻2𝑆𝑂4 𝑥 𝑁 𝐻2𝑆𝑂4) −]𝑥 𝑚𝐸𝑞 𝑤𝑡 𝑜𝑔 𝑀𝑔 (𝑂𝐻)2 CUVETTE
=
𝑤𝑡. 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 𝑖𝑛 (𝑔) - In spectroscopy, a cuvette (also known as a
spectrophotometer cell) is a small,
CHEMICAL REACTION OF MAALOX WITH H2SO4 rectangular, transparent container used to
AND EXCESS OF NaOH hold a sample for analysis by a
H2SO4 + Mg(OH)2 → MgSO4 + 2H2O spectrophotometer
- In this reaction, sulfuric acid reacts with - Is then placed inside the spectrophotometer
magnesium hydroxide in the MoM to form where the light passes through the sample
Magnesium Sulfate and water and the amount of light absorbed is measured
- At the equivalence point, all of the excess sulfuric - Designed to be optically clear and have flat,
acid has been neutralized, and the amount of parallel surfaces to minimize light scattering
NaOH used in the titration can be used to and ensure accurate measurements
calculate the amount of MoM present in the SPECTROPHOTOMETER
sample - An instrument that measures the intensity of
light absorbed by a sample at different
SPECTROCHEMICAL ANALYSIS wavelengths, and is used to determine the
- Refers to techniques for chemical analysis that concentration of a substance in the sample
rely on the measurement of electromagnetic
radiation's wavelength and intensity. BEER’S LAW
- On the basis of the amounts of energy absorbed - The relationship between absorbance and
during changes in the structure or motion of the concentration in a sample is described by the
molecules, it is mostly used to determine the Beer-Lambert Law,
arrangement of atoms and electrons in - States that the absorbance of a sample is directly
molecules of chemical compounds. proportional to its concentration and the path
- Two techniques—ultraviolet (nonvisible) and length of the light through the sample
visible emission spectroscopy and ultraviolet, - This relationship means that as the concentration
visible, and infrared absorption of a sample increases, its absorbance will also
spectrophotometry—are typically indicated in its increase
more restricted and widespread employment

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Mathematically, this law can be expressed as: - The more polar component travels slower
A = εcl / A=abc SILICA GEL AND ALUMINA
- The most used solid adsorbents as
Where: stationary phases in laboratory due to
A = absorbance their versatile polarity range
ε = molar absorptivity or extinction coefficient (a - The solid phase (silica gel or alumina) is
constant that depends on the properties of the applied as a thin coating on a plastic sheet
sample and the wavelength of light used) or glass slide, called a TLC plate
c = concentration of the sample .PROCEDURE OF TLC PLATE
l = path length of the light through the sample 1. Draw a horizontal line about 1 cm from the
(usually measured in centimeters) bottom of the TLC plate to mark the starting point
of the sample for elution
BLANK SOLUTION 2. Add 4 hash marks (reference lanes) perpendicular
- A blank solution, also known as a reference to line
solution, is a solution that does not contain the 3. Carefully spot small amounts of analytes (sample
analyte of interest but is otherwise identical to solutions) on the reference lanes
the sample being analyzed
- Used to calibrate the instrument and to correct REFERENCE A Methylene Blue
for any background signals that may interfere REFERENCE B Methyl Red
with the measurement of the sample REFERENCE C Methyl Orange
REFERENCE D Dye Mixture
THIN LAYER CHROMATOGRAPHY (TLC)
CHROMATOGRAPHY - Three (3) or four (4) applications of the
- Is a technique used for the analysis and same solution should suffice to produce a
separation of chemical mixtures good spot
- The technique is based on a polarity interplay - Precaution: Avoid making big or large
between the sample and two other spots, therefore just “peck” the coating
substances called the solid or stationary and withdraw the spot applicator or
phase and the mobile phase or eluent, which toothpick.
can be a liquid or a gas 4. While the spots are being applied and allowed to
- As their names indicate, the stationary phase dry, prepare a developing chamber for the
does not move, whereas the mobile phase separation.
flows across, or through the solid phase a.) Prepare an eluting solvent (eluent). Mix 3.6
- The sample to be separated first becomes mL of Ethanol and 3.6 mL of Acetone in a 10-
adsorbed onto the surface of the solid phase mL graduated cylinder
through polar interactions b.) Transfer the eluting solvent into the 250-mL
- The more polar the solvent, the greater its beaker carefully
capacity to carry the components of the c.) Take a piece of filter paper and place it around
mixture with it, “yanking” them away from the inside walls of the beaker that it is soaked
the solid phase as it moves with the solvent, or you may squirt some of
- Different components with different the eluting solvent on the filter paper to make
polarities will travel at different rates as the it wet so that it adheres to the beaker walls
solvent moves, causing their separation better
- The less polar component travels faster d.) Cover the beaker with a watch glass while
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waiting for the TLC plate

e.) Once the TLC plate has been completely
spotted and dried, carefully place it inside the
beaker using a tweezer. The TLC plate should
be placed upright, slightly inclined against the
wall of the beaker.
- Precaution: the solvent should not touch
the spots, that’s why its level should be
below the spots by at least 0.5 cm
f.) Cover the beaker with a watch glass and wait
for the elution to proceed. As the solvent
moves up to the TLC plate, it will cause the
spots to move as well
5. When the solvent front is about 0.5 to 1 cm from
reaching the top of the TLC plate, it is time to stop
the elution. Do not allow the solvent to reach the
top of the plate
- Precaution: If you wait too long, it will
fade, and you will miss a crucial part of
information needed to calculate the Rf
values
6. Compute the retardation or retention factor
values (Rf values) of the following spots. These
can be calculated using the formula below

𝑑𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙𝑒𝑑 𝑏𝑦 𝑡ℎ𝑒 𝑠𝑝𝑜𝑡

𝑅𝑓 =
𝑑𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙𝑒𝑑 𝑏𝑦 𝑡ℎ𝑒 𝑠𝑜𝑙𝑣𝑒𝑛𝑡 𝑓𝑟𝑜𝑛𝑡

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