ACTIVITY # I-Loss on Drying

Loss on drying is a widely used test method to determine the

moisture content of a sample, although occasionally it may refer
to the loss of any volatile matter from the
sample. Loss in drying does not usually refer to molecularly
bound water or water of crystallisation
LOD is used to determine the amount of water that will vaporize
under given or specified conditions such as temperature,duration
time, or in vacuum using specified apparatus such as
pharmaceutical oven.

Pharmaceutical oven

Toluene distillation

2 methods in determining water content

1.titrimetric method –using Karl Fischer Reagent =in which
sulphur dioxide and iodine are dissolved in pyridine and
methanol
Titrimetric analysis

Karl fischer method

2.Azeotropic- Toluene distillation method

In chemical engineering, azeotropic distillation usually refers to
the specific technique of adding another component to generate
a new, lower-boiling azeotrope that is heterogeneous (e.g.
producing two, immiscible liquid phases), such as the example
below with the addition of benzene to water and ethanol

3.Gravimetric method-
Gravimetric analysis is a technique through which the amount
of an analyte (the ion being analyzed) can be determined
through the measurement of mass. Gravimetric analyses
depend on comparing the masses of two compounds containing
the analyte.

Computation :
% Loss on drying = ((B-C)-A) x 100
​ ​ ​(B-A)

The presence of water plays an important role in the physical

and chemical stability of the active pharma-
ceutical ingredients, and pharmaceutical preparations, because
they may lead to their degradation. Water in pharmaceutical
substances and preparations, provides a favorable environment
for bacterial growth

ACTIVITY # 2
MOISTURE CONTENT-MOISTURE ANALYZER

Moisture analyzer offers reliability and simplicity to measure he

moisture content of samples ranging from powders to liquids.
This combination of internal balance and infrared dryer provides
results in 5 to 15 minutes on average.Percent moisture are usuall
calculated to 0.01% resolution

Moisture Analyzer
The measurement principle does not differ from that of the
thermogravimetric method. The main distinction lies with the
type of heat source used: In the oven, samples are heated by
convection while a moisture analyzer heats samples via the
absorption of infrared energy.

ACTIVITY # 3
REFRACTIVE INDEX – REFRACTOMETER

If the light enters the denser substance at an angle, one part of

the wave slows down more quickly as it passes the interface. It
produces a bending of the wave toward the interface which is
called Refraction . The relative value of the effect of refraction
between two substances is given by the Refractive index of as
substance which, is the ratio of the velocity of light in air to the
velocity of light in the substance. The refractive index can be
used to identify a substance, to measure its purity or detection of
impurities. Refractometer is used to determine refractive index,
which varies with the wavelength of light and the temperature.
The temperature as specified depending on the substance, should
be carefully adjusted and maintained.

The Abbe Refractometer measures the range of refractive index.

For theoretical accuracy, it is necessary to calibrate the
instrument against a standard provided by the manufacturer of
refractometer and check the temperature control and cleanliness
of the instrument by determining the refractive index of distilled
water, which is 1.3330 at 20degrees and 1.3325 at 25degrees.

Pharmaceutical Refractometers. The refractive index (RI)

is used to determine the purity of a sample. Refractometers are
often used in pharmaceutical applications for quality control
of raw intermediate and final products

Application Need: There is an important need and requirement

for measuring the refractive index value of various
pharmaceutics. Refractive index (RI) is used to determine the
purity of the sample. Pharmaceutical manufacturers must
measure the RI of raw materials before placing them into their
production schedule. In addition, the R&D and QC Laboratories
may need to measure the RI of the pharmaceutical product to
monitor reaction changes.
The Problem: The manual, or Abbe refractometer, projects a
visible shadowline on the crosshairs in the instrument. This
shadowline is often blurry. Operator misinterpretation of the
shadowline can result in significant measurement errors. Also,
RI is temperature dependent. In order to standardize readings,
they must be either controlled or corrected to a standard
reference temperature (typically 20 or 25 per the US and EU
Pharmacopoeia).
The Solution: Reichert automatic digital refractometers are
ideal for measuring RI. Here is why: ✓ Sample color or opacity
does not effect automatic refractometers. Fully automatic
refractometers are also known as reflected light refractometers
because they utilize the light that is reflected by the sample for
analysis. ✓ Reduced operator error. An electronic detector is
used instead to take the measurement. ✓ Temperature may be
controlled via an external water bath circulator on the AR6
Series, ARIAS, and MARK models, or by a built in Peltier
Thermal Control System on the AR7 Series. ✓ To ensure the
refractometer and sample have stabilized at a given temperature,
the AR7 Series, AR6 Series, ARIAS, and MARK III
refractometers utilize an exclusive feature known as Automatic
Temperature Equilibration Detection.
ACTIVITY # 4

In chemistry, specific rotation ([α]) is a property of a chiral chemical compound. It is defined as

the change in orientation of monochromatic plane-polarized light, per unit distance–
concentration product, as the light passes through a sample of a compound in solution

Types of polarimeter
Laurent's Half-Shade Polarimeter. It is used for the
measurement of the angle of rotation of optically active
substance in solution. That is, angle through which the plane of
the polarized light is rotated on passing through a specific length
of solution of known concentration

Biquartz's Polarimeter is a polarimeter which can be used to

determine specific rotation more accurately.And also used to
measure the angle of rotation of plane of polarisation rotated by
an optically active substance.Bi-Quartz plays a crucial role in
the experiment of specific rotation using polarimeter

Lippich polarimeter
Laurent’s polarimeter suffers from the defect that it can be used
only for light of a particular wavelength for which the half wave
plate has been constructed. To overcome this difficulty, Lippich
constructed a polarimeter, that can be used for light of any
wavelength.

ACTIVITY # 5
Bottle and closure inspection

A caliper (British spelling also calliper, or in plurale tantum

sense a pair of calipers) is a device used to measure the distance
between two opposite sides of an object. Many types
of calipers permit reading out a measurement on a ruled scale, a
dial, or a digital display.

Types of closures:
a.biological
b.brandy cork
c.shallow CT
d.Pry off
e.Roll on
f.Pilfer proof

Critical defects
-bird-swings &spikes
-overpress
-filament
-split
-check
-poor distribution
-soft blister
-cracks
-pinholes
-chipped finish
-contamination

Major defects
-stone
-rocker bottom
-mismatch
-fin
-out of round finish

Minor defects
-tear
-washboard
-hard blister
-heeltap
-seeds

Activity # 7
pH Determination

A potentiometer is a three-terminal resistor with a sliding or

rotating contact that forms an adjustable voltage divider. If only
two terminals are used, one end and the wiper, it acts as a
variable resistor or rheostat
The major disadvantage is that it requires a large force to move
their sliding contacts i.e. wiper. There is wear and tear due to
movement of the wiper. It reduces the life of this transducer

Advantage:It gives sufficient output that does not require further

amplification. They are useful for the measurement of large
displacement. The resolution is infinite in cermet and metal
film potentiometers

table top pH meter

Potentiometry- is defined as a branch of electrochemistry which
deals with the study and measurement of electrode potentials.
When hydrogen ion concentration is determined with a
laboratory device such as potentiometer or pH meter equipped
with electrodes, one actually measures the activity o the
hydrogen ion. The glass electrode is the most popular o all
indicator electrodes for pH determination because o the high
electric resistance of the glass.Almost all glass electrode have
sufficient properties for working in the pH meter when properly
standardized is capabale o reproducing pH values to 0.02.
Measurements are amde at 25+ 2degrees unless other conditions
are specified.

Prior to daily use standardization of the pH meter is to be done.

Buffer solution or standardization are prepared or buffer salts of
required purity can be obtained from the National Institute of
Science and Technology (NIST). Fresh solutions should be
prepared at intervals not to exceed 3 months using carbon-
dioxide free water and stored in hard glass or polyethylene
bottles fitted with a tight closure.

ACTIVITY # 10

Analytical balance

Analytical balances are highly sensitive lab instruments

designed to accurately measure mass. Their readability has a
range between 0.1mg - 0.01mg. Analytical balances have a
draft shield or weighing chamber to prevent the very small
samples from being affected by air currents.

Top-loading balances, which can measure objects up to 200 g,

are less expensive but less exacting than analytical balances.
They are considered semi-analytical balances, with a
readability of up to three decimal places to the right of the
decimal point (up to .001 g). Precision balances have a
readability of 0.01 g.
Weight variation was carried out to ensure that, each of tablets
contains the proper amount of drug. The test was carried out by
weighing the 20 tablets individually using analytical balance,
then calculating the average weight, and comparing the
individual tablet weights to the average

Activity # 12

Activity # 13
Tablet friability

Friability (the condition of being Friable) testing is a method,

which is employed to determine physical strength of compressed
and uncoated tablets upon exposure to mechanical shock and
attrition. ... The strength of a tablet plays a very important role
in its marketing and dissolution

Activity # 14
Tablet Hardness
The application of hardness testing enables you to evaluate a
material's properties, such as strength, ductility and wear
resistance, and so helps you determine whether a material or
material treatment is suitable for the purpose you require

Actvity # 15
Significance of disintegration test
Disintegration is an important quality control test today. In the
future, disintegration testing could become a release test for
formulations with API-controlled dissolution. ... In order to
harmonize the disintegration test throughout the different
pharmacopeias, many specification changes have been made in
the USP

It is a measure of the time required under a given set of

conditions for a group of tablets to disintegrate into particles
which will pass through a 10 mesh screen. The test is useful as a
quality assurance tool for conventional dosage forms

Activity # 16
Dissolution testing is an in vitro method that characterizes how
an API is extracted out of a solid dosage form. It can indicate the
efficiency of in vivo dissolution but does not provide any
information on drug substance absorption.

Activity # UV-VIS Spectrophotometer

Ultraviolet–visible spectroscopy or ultraviolet–visible

spectrophotometry refers to absorption spectroscopy or
reflectance spectroscopy in part of the ultraviolet and the
full, adjacent visible spectral regions. This means it uses
light in the visible and adjacent ranges

Liquid chromatography
Liquid chromatography (LC) is an
analytical chromatographic technique that is useful for
separating ions or molecules that are dissolved in a solvent.

Speed, Efficiency and Accuracy

Compared to other chromatographic techniques, such as TLC,
HPLC is extremely quick and efficient. It uses a pump, rather
than gravity, to force a liquid solvent through a solid adsorbent
material, with different chemical components separating out as
they move at different speeds.

High-performance liquid chromatography is a technique in

analytical chemistry used to separate, identify, and quantify each
component in a mixture. It relies on pumps to pass a pressurized
liquid solvent containing the sample mixture through a column
filled with a solid adsorbent material. Wikipedia
Analytes: organic molecules; biomolecules; ions; polymers

Speed, Efficiency and Accuracy. Compared to other

chromatographic techniques, such as TLC, HPLC is extremely
quick and efficient. It uses a pump, rather than gravity, to force a
liquid solvent through a solid adsorbent material, with different
chemical components separating out as they move at different
speeds

Disadvantages & Advantages of an HPLC. HPLC and Similar

Techniques. Like other forms of chromatography, HPLC allows
the separation of chemical constituents through the use of a
mobile phase and a stationary phase