Topic Coverage

●
Raw Material Testing
●
Packaging Material Testing
●
Finish Product Testing

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Raw Material Test Procedure
1.Loss on Drying
2.Moisture Content
3.Refractive Index
4.Optical Rotation

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
LOSS ON DRYING
Many Pharmaceutical ingredients or raw
materials are hydrates or contain water.
Water Content determination is important in
compliance with the Quality Control Raw
Material Evaluation or screening.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
LOSS ON DRYING
There are different methods in determining
water content. These include:
●
1) Titrimetric Method using Karl Fischer
Reagent, in which the sulfur dioxide and
iodine are dissolved in pyridine and
methanol;
●
2) AzeotropicToluene Distillation Method,
●
3) Gravimetric method such as loss on
drying
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
LOSS ON DRYING
Loss on drying 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.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 1: LOSS ON DRYING
OBJECTIVE:
To be able to perform and determine the
water content of substances using the
gravimetric method - loss on drying.
APPARATUS:
Weighing bottle, analytical balance,
spatula, oven or as specified, desiccator.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 1: LOSS ON DRYING
PROCEDURE:
1. Mix and accurately-weigh the substance-to
be tested, and, unless otherwise directed in
the individual monograph, conduct the
determination on 1 to 2g of sample. If the test
specimen is in the form of large crystals,
reduce the particle size to about 2mm by
quickly crushing.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 1: LOSS ON DRYING
PROCEDURE:
2. Tare a weighing bottle that has been
washed thoroughly and dried for 30 minutes
same with the conditions to be used with the
material, but has been cooled to room
temperature in the desiccator.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 1: LOSS ON DRYING
PROCEDURE:
3. Put the material in the weighing bottle and
accurately weigh the weighing bottle with the
contents.
4 Uniformly distribute the material using a
spatula, and cover.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 1: LOSS ON DRYING
PROCEDURE:
5. Put the weighing bottle in the oven which
is set at and meets the required conditions,
removing the cover, leaving the cover in the
Oven.
6. Dry the material at the temperature and
time or l and with other required conditions.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 1: LOSS ON DRYING
PROCEDURE:
7. Then, open the oven, cover immediately
the weighing bottle and allow to cool to room
temperature in the desiccator.
8. Weigh the weighing bottle with content.
9. If specimen under test is capsule; use a
portion of the mixed contents of not less than
4 capsules.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 1: LOSS ON DRYING
PROCEDURE:
10. If specimen under test is tablet, use
powder from not less than 4 tablets, ground
to a fine powder.
11. Where drying in vacuum over a desiccant
is directed, a vacuum desiccator is to be
used. Ensure the desiccant is kept fully
effective by frequent replacing

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 1: LOSS ON DRYING
PROCEDURE:
12. After gaining the room temperature,
weigh and compute the percentage loss on
drying.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 1: LOSS ON DRYING
Data & Result:
Weight of the weighing bottle (A) : ________
Weight of the weighing bottle & content (before drying) (B): _______
Weight of the weighing bottle & content (after drying) (C): ________
Computation:
% Loss on drying = ((B-C) – A) x 100
(B - A)

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 1: LOSS ON DRYING
Conclusion:

Question: What is/are the importance of determining the water

content of Pharmaceutical raw materials/ product?

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
MOISTURE CONTENT-MOISTURE ANALYZER
The Moisture analyzer offers reliability and
simplicity to measure the moisture content
of samples ranging from powders to liquids.
This combination of an internal balance and
an infrared dryer provides results in 5 to 15
minutes on average. Percent moisture are
usually calculated to 0.01% resolution. O'haus Moisture Analyzer

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 2. Moisture Content using Moisture Analyzer
Objective:
To be able to familiarize, perform and determine the moisture content
of a substances using a moisture balance.

APPARATUS/ GLASSWARE:
O'haus Moisture balance, or any brand, spatula

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 2. Moisture Content using Moisture Analyzer
PROCEDURE
CAUTION Moisture balances have no ventilation so all the
fumes remain inside the hood of the moisture balance. Ask your
instructor prior to using any moisture balances for your safety.
1. Turn the moisture balance ON by pressing the ON/OFF button
located at the upper left corner of the control panel. The display
indicates the parameters set for moisture analysıs.
2. Open the cover of the moisture analyzer.
3 Clear the pan.
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 2. Moisture Content using Moisture Analyzer
4. Place the empty sample pan in the panhandler (this is possible
without tilting the sample pan if you insert this in the pan handler from
the side directly below the round flange)
5. Place the panhandler in the sample chamber. Ensure that the
tongue of the panhandler fits exactly in the slot of the draft shield
element. The sample pan must lie flat in the panhandler.
6. Press the tare button. This sets the moisture analyzer to zero.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 2. Moisture Content using Moisture Analyzer
7. Place the specimen sample in the sample pan. (Set at 5 g)
8. Close the cover.
9. Press the START/STOP button. The moisture analyzer starts the
drying and measurement process.
10. The test automatically stops at the end of the time set for the
test (eight minutes), record the result.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 2. Moisture Content using Moisture Analyzer
11. Carefully remove the sample panhandler from the drying area.
12. Remove the sample pan from the panhandler.
13. Turn off the unit by pressing the ON/OFF button located at the
upper left corner of the display panel.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 2. Moisture Content using Moisture Analyzer
Data and Result:
Conclusion:
Questions:
1. Sketch the moisture balance and label its parts.
2. What are advantages of this method over other methods
of moisture determination?

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
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 a
substance which, is the ratio of the velocity of light in air to
the velocity of light in the substance.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
REFRACTIVE INDEX-REFRACTOMETER
The relative value of the effect of
refraction between two
substances is given by the
REFRACTIVE INDEX of a
substance which, is the ratio of
the velocity of light in air to the
velocity of light in the substance.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
REFRACTIVE INDEX-REFRACTOMETER
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 cleanliness
of the instrument by determining the
refractive index of distilled water, which is
1.3330 at 20° and 1.3325 at 25°

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 3. REFRACTIVE INDEX-REFRACTOMETER
OBJECTTVE: To be able to determine the refractive index of
a substance using a handheld refractometer.

APPARATUS / GLASSWARE: Refractometer

MATERIAL/ SAMPLE: Distilled water, any liquid flavor or any
liquid sample

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 3. REFRACTIVE INDEX-REFRACTOMETER
PROCEDURE
1. Open the illuminator flap.
2. Put a sample on the measurement prism surface, using
dropper or pipette.
3. Close the flap.
4. Look through the eyepiece.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 3. REFRACTIVE INDEX-REFRACTOMETER
PROCEDURE
5. Read result from the scale, if necessary place the
refractometer in the direction of light.
6. Wipe dry the prism and flap with a clean, soft cloth.
7. Perform in two trials.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 3. REFRACTIVE INDEX-REFRACTOMETER
Determine the Refractive Index:
Reference use: https://pubchem.ncbi.nlm.nih.gov/

Substance Refractive Index

1. Salicylic Acid

2. Peppermint Oil

3. Menthol

4. Acetic Acid

5. Glycerol

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 3. REFRACTIVE INDEX-REFRACTOMETER
Questions:
1. What are the specific use/s of a refractometer in
pharmacy?
2. Draw the handheld refractometer and label its parts.
3. What is an Abbe refractometer? Draw and label the parts.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
OPTICAL ROTATION - POLARIMETER
OPTICAL ROTATION means that the polarization of the
direction of light will be rotated for a certain angle when
penetrating an optically active substances.
According to the direction in which the light is rotated, the
optically active substance is referred to as, dextrorotatory
designated as (+), clockwise rotation (to the right) or
levorotatory designated as (-), counterclockwise rotation (to
the left)

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
OPTICAL ROTATION - POLARIMETER
POLARIMETER is used to measure the
optical rotation of plane polarized light
when illuminating an optically active
substances, such as sugar solutions,
turpentine oil and camphor. It is use to
determine the rotatory power or lack of
rotatory power of a substance, which
serves as its identity, purity and its
measurements indicates the therapeutic
value.
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
OBJECTTVE: To be able to identify the
parts of a polarimeter and determine the
specific rotation of a sugar solution.
APPARATUS/ GLASSWARES
Volumetric flask, weighing balance,
polarimeter, others (as needed)
MATERIAL/ SAMPLE: Sucrose solution

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
PROCEDURE
1. SAMPLE PREPARATION
A)THE SPECIFIC ROTATION OF SUCROSE
1. Weigh as accurately as possible about 52 grams of sucrose.
2. Dissolve it in enough distilled water to make a 100mL solution.
3. Transfer 50mL of the solution into a 100mL volumetric flask, and
dilute to the mark with distilled water. Mix the solution well. Cool.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
4. Optical rotation is determined within 30 minutes after the
preparation at 250 ± 0.5°C
5. Carefully rinse the sample tube twice with this solution.
6. Obtain 3 readings of this solution and get the average. Average
optical rotation of sucrose:________
7. Calculate the specific rotation of sucrose.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
B) THE INVERSION OF SUCROSE
1. Clean and rinse well the volumetric flask used above.
2. Place the other 50ml portion of the prepared sucrose solution in the
clean volumetric flask.
3. Add 25mL of distilled water and 5mL of conc. HC1
4. Heat in a water bath for 15 minutes, keeping the temperature
constant at 70°C
5. Cool thoroughly under running water.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
6. Add drop by drop saturated NaOH solution, shaking after each
addition until a drop of the solution gives a pink color to
phenolphthalein which is used as an outside indicator.
7. Dilute to the mark with distilled water and mix thoroughly.
8. Rinse the sample tube twice.
9. Obtain 3 readings of this solution and get the average. Average
optical rotation of sucrose:_______
10. Calculate the specific rotation of sucrose.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
2. USING THE APPARATUS
1. Pour the solution to be measured into the test tube for
measurement.
Caution: the screws at the both ends of the test tube should not to be
tightened more than necessary.
2. Connect the power source and switch on the sodium lamp. Wait for
about 10minutes until the lamp emits yellow sodium light.
3. Rotate the scale knob until the illumination of the viewing field have
equal intensity
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
4. Check the zero-position of the vernier scale. If the position is not in
zero adjustment can be made or adjust to zero position.
5. Open the cover of the sample chamber, and put the test tube into
the chamber, the bulb part of the test tube is in upward position.
6. Adjust the viewing field screw until the triplex viewing aspect
becomes distinct.
7. Rotate the scale knob until illumination of the viewing field becomes
identical.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
8. Read on the dial, thru a magnifying glass, the angle of rotation.
9. After using clean the apparatus.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER

α= a
(l)(c)

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
Optical Rotation Computation:
Given:
1. A sample of pure 2-butanol was placed in a 10cm polarimeter tube.
Using the D-line of a sodium lamp, the observed rotation at 20°C was
a= +104°. The conc. of the compound is 0.805 g/ mL.
What is the specific rotation of 2-butanol?

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
Optical Rotation Computation:
Given:
2. Calculate the observed rotation of a solution of 5.245 g of 1-
ammonium-1-phenylethane diluted to a volume of 100 mL w/ a
methanol at 20°C using the D-line of a sodium lamp and a 1 dm tube.
Specific rotation of this material=(-30°)
Sample concentration is 5.245 g in 100mL

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
Optical Rotation Computation:
Given:
3. Calculate the specific rotation of 2,3-tartaric acid based on the ff
observation:
A 0.856 g sample of pure acid was diluted to 10 mL w/water and
observed in a 1.00 dm polarimeter tube. The observed rotation using
the 589 nm line of a sodium lamp at 20°C was a=+1.06.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 4. OPTICAL ROTATION - POLARIMETER
Question:
1. What is meant by specific rotation?
2. Enumerate and differentiate the type of polarimeter.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Packaging Material Test Procedure
1. Bottle and Closure Inspection
2. Inspection of labels and box

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
BOTTLE AND CLOSURE INSPECTION
Bottle is one of the primary packaging materials of
pharmaceutical products. Inspection and evaluation are to be
done prior to use, from its physical attributes to
microbiological tests. One of the physical evaluations to be
done is to visually check the presence of bottle defects,
which are classified as critical defects, major defects and
minor defects.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
BOTTLE AND CLOSURE INSPECTION
Critical defects are defects which prevent the glass bottle
from performing their intended function of safely holding the
product. These may cause danger to consumers.
Major defects are defects that make handling of the bottle
difficult. In this case, bottle durability is questionable.
Minor defects are defects which adversely affect the
appearance but not the function of the bottle.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
BOTTLE AND CLOSURE INSPECTION
Also, in taking the required measurements of bottle such as
height and diameter, a vernier caliper is used. Shown in the
figure below, are parts of vernier caliper.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
BOTTLE AND CLOSURE INSPECTION

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 5. BOTTLE AND CLOSURE INSPECTION
OBJECTIVE:
To identify and describe the different kinds of closures and to
identify and classify different bottle defects
APPARATUS/ GLASSWARE: Vernier caliper, graduated
cylinder
MATERIALS/ SAMPLES: Different samples of closures,
different samples for different bottle defects, 10 pieces of
closure in similar type, 10 bottles in similar type.
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 5. BOTTLE AND CLOSURE INSPECTION
PROCEDURE:
A. Types of Closures
1. Draw the bottle finish design listed below, and identify and
draw the closure most suitable for each design.
a. Biological d. Pry off
b. Brandy cork e. Roll on
c. Shallow CT f. Pilfer proof
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 5. BOTTLE AND CLOSURE INSPECTION
2. Inspect ten (10 pcs.) cap or closure of similar type.
3. Identify using the above types of closures, metal screw
cap or plastic.
4. Check if cap liners are present.
5. Measure the inner or outer diameter. (in mm)

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 5. BOTTLE AND CLOSURE INSPECTION
B. Inspection of Bottle
1. Inspect ten (10 pcs.) bottles of similar type.
2 Describe the bottle in terms of color, type of mouth of bottle
and its capacity.
3. Check and average the fill volumes (in mL), inner and
outer diameters (in mm) of its mouth and depth or height of
the bottles (in mm) of the 10 bottles.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 5. BOTTLE AND CLOSURE INSPECTION
4. Check the bottles for presence of any defects, such as:
a. Critical defects
Bird-swings and spikes Overpress Pinholes
Filament Split
Check Poor distribution
Soft blister Cracks
Chipped finish Contamination of foreign materials
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 5. BOTTLE AND CLOSURE INSPECTION
b. Major defects c. Minor defects
Stone Sunken (dropped shoulder)
Rocker Bottom Tear
Mismatch Washboard
Fin Hard blister
Out of round finish Heeltap
Seeds
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 5. BOTTLE AND CLOSURE INSPECTION
Data and Result:
A) Picture of types closures

B) Pictures of different defects (critical, major & minor)

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 5. BOTTLE AND CLOSURE INSPECTION
C) Data Table: Sample No. Presence of Cap
liner
Inner Diameter
(mm)
Outer Diameter
(mm)
1.
CLOSURE 2.
3.
For the computation: 4.
A. Average inner diameter
5.
B. Average outer diameter
6.
7.
8.
9.
10.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 5. BOTTLE AND CLOSURE INSPECTION
C) Data Table: Sample
No.
Fill Volume
(ml)
Inner Diameter
(mm)
Outer Diameter
(mm)
Height
(mm)
1.
BOTTLE 2.
3.
For the computation: 4.
A. Average Fill vol.
5.
B. Average Inner diameter
C. Average Outer diameter 6.
D. Average height 7.
8.
9.
10.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 5. BOTTLE AND CLOSURE INSPECTION
C) Data Table: Sample
No.
Deffects Classification

DEFFECT

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Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
INSPECTION OF LABEL AND BOX
Packaging materials are checked and inspected prior to use,
using Packaging Material Specification or comparing it with
the standard. Inspection starts from the receiving area up to
the point of use, to avoid mix-ups and mislabeling.
In the receiving area, the type of the container used to pack
the bulk of packaging materials, its integrity, cleanliness and
the presence of label are inspected.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
INSPECTION OF LABEL AND BOX
Packaging materials are classified as primary and
secondary packaging materials. Primary packaging
materials are those which come in direct contact with the
product itself. These includes bottles, cap or closures, foil or
aluminum foil and tubes. Secondary packaging materials are
those which do not come in direct contact with the product
and serve as accessory to the primary packaging materials,
such as label, individual boxes, insert and corrugated boxes
or shippers.
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
OBJECTTVE: To be able to inspect secondary packaging
materials, labels and individual boxes.
APPARATUS/ GLASSWARE: Vernier caliper
MATERIALS/ SAMPLES : 10 pieces of label, 10 pieces of
boxes

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
PROCEDURE:
A. Inspection of Labels
1. Inspect the ten (10 pieces) of labels
2. Check the following:
● printed text
● color using the color guide (pantone color)
● size of generic box

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
● font size of generic name is one size bigger than the
brand name
● font style and background of generic and brand name are
the same
● size of the Rx symbol (at 1/5 of the height of the label)
● data regarding the product should reconcile with the insert
(if present)
● company logo, name and address

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
3. Measure the dimensions, width and height, appropriate to
the bottle size, thickness of the label.
B. Inspection of Boxes
1. Inspect the ten (10 pieces) of boxes
2. Check the following:
● printed text
● color using the color guide (pantone color)
● size of generic box
● font size of generic name is one size bigger than the brand
● name
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
● font style and background of generic and brand name are the
● same
● size of the Rx symbol (at 1/5 of the height of the label)
● data regarding the product should reconcile with the insert (if
● present)
● company logo, name and address
● enough gluing
● bottom lock-easily open, if present

4. Measure the dimensions, width and height, appropriate to the

bottle size and thickness of the boxes.
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
Data & Result:
A. Inspection of Label
Labels (Check if similar with the standard or according to
requirements)
[ ] printed text
[ ] color using the color guide (pantone color)
[ ] size of generic box _____mm
[ ] font size of generic name is one size bigger than brand
name
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
[ ] font style and background of generic and brand name are
the same
[ ] size of the Rx symbol (at 1/5 of the height of the label)
[ ] data regarding the product shoukd reconcile with the box
and insert
[ ] company logo, name and address
[ ] dimensions: { } width ___ mm { } height ___ mm
{ } thickness ___ mm
Findings and Remarks: ____________________________
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
B. Inspection of Box
Boxes (Check if similar with standard or according to
requirements)
[ ] printed text
[ ] color using the color guide (pantone color)
[ ] size of generic box___ mm
[ ] font size of generic name is one size bigger than brand
name

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
B. Inspection of Box
Boxes (Check if similar with standard or according to
requirements)
[ ] printed text
[ ] color using the color guide (pantone color)
[ ] size of generic box___ mm
[ ] font size of generic name is one size bigger than brand
name

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
[ ] font style and background of generic and brand name are
the same
[ ] size of the Rx symbol (at 1/5 of the height of the label)
[ ] data regarding the product shoukd reconcile with the box
and insert
[ ] company logo, name and address
[ ] dimensions: { } width ___ mm { } height ___ mm
{ } thickness ___ mm
Findings and Remarks: ____________________________
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 6. INSPECTION OF LABEL AND BOX
QUESTION/S:
1. What is Packaging Material Specification?
2 What is the meaning of "principal display panel"? Give
details needed to be indicated in the principal display panel?
3. Give at least 10 drug products that require the "Rx"
symbol to be indicated on its label and box.
4. Give at least 10 drug products that do not require the "Rx
symbol to be indicated on its label.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Finish Product Test Procedure
● pH Determination
● Deliverable Volume
● Homogeneity Test
● Analytical Balance
● Weight Variation
● Tablet Thickness and Diameter
● Tablet Friability
● Tablet Hardness/ Tablet Breaking Force
● Disintegration Test
● Dissolution Test
● UV-VIS Spectrophotometer
● Liquid Chromatography
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
pH DETERMINATION
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 a potentiometer or a pH meter
equipped with electrodes, one actually measures the activity
of the hydrogen ion.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
pH DETERMINATION
The glass electrode is the most
popular of all indicator electrodes for
pH determination because of the high
electric resistance of the glass.
Almost all glass electrode have
sufficient properties for working in the
pH range from pH 2 to pH 12.

PH Meter Table Top Bench type

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
pH DETERMINATION
This potentiometric instrument or pH meter when properly
standardized is capable of reproducing pH values to 0.02.
Measurements are made at 25 ± 20°, unless other
conditions are specified.
Prior to daily use, standardization of the pH meter is to be
done. Buffer solution for standardization are prepared or
buffer salts of required purity can be obtained from the
National Institute of Science and Technology (NIST).

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
pH DETERMINATION
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.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
OBJECTIVE: To be able to prepare buffer solutions for pH
meter standardization, and perform the standardization
process, and determine the pH of pharmaceutical product.

APPARATUS / GLASSWARE pH meter (either portable or

table top), wash bottle

MATERIALS/SAMPLES: Buffer solutions, any

pharmaceutical liquid product
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
PROCEDURE:
A. Preparation of buffer solutions

1.Buffer solution 4.0 is 0.05 m potassium biphthalate.

Prepare Buffer solution 4.0 by dissolving 10.12 g of
potassium biphthalate, previously dried at 110° for l hour,
in carbon dioxide-free water to make 1000 mL.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
PROCEDURE:
A. Preparation of buffer solutions

2. Buffer solution 7.0 is 0.05 m equimolal phosphate.

Prepare Buffer solution 7.0 by dissolving 3.53 g of
disodium hydrogen phosphate and 3.39 g of monobasic
potassium phosphate. Each previously dried at 120° for 2
hours, in carbon dioxide-free water to make 1000 mL.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
B. Standardization/calibration of pH meter
Note: This procedure is for the table top pH meter, minimal
adjustment for the portable pH meter.
1. Calibrate the pH meter prior to use. A two-point calibration is to be
done, depending on the pH to determine. (ex. Sample has pH 5.0,
calibration using buffer solution pH 4.0 and buffer solution pH 7.0 is
to be used)

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
2. Select the pH mode using the MODE key. Rinse the electrode well
with distilled water or rinse solution. (CAUTION: Do not wipe the
electrode as this may cause a build-up of electrostatic charge on the
glass surface!)

3. Immerse the electrode into the standard buffer to be calibrated

and press the CAL key to calibrate the meter. The display will show
the [CAL] mode, the secondary display will indicate that pH 7.00 is
ready for calibration. Wait for the pH value to stabilize. The ready
indicator will appear when reading has stabilized.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
4. Select the second desired buffer value or pH 4.00 using the ↑↓
keys. Then calibrate.
5. Press CON key when ready indicator appears. The CON indicator
flashes for one second and disappears. Upon confirmation, the
instrument is calibrated to the buffer indicated in the secondary
display.
Note: The buffer, ERR and electrode annunciator flashes if
selected buffer value is not within ± 0.50 pH from the measured
pH Value

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
6. Press MEAS key to return to the measurement mode. Ready to
use.
7. In the presence of automatic temperature compensator (ATC), in
this calibration procedure, the ATC probe is attached to the meter
and the ATC annunciator is lighted up on the right hand side of the
LCD. Press the MODE key to select temperature mode [Temp].
Make sure that you are in the [MEAS] mode prior to commencement.
8. Go to the calibration mode, press the CAL. The primary display
indicates the measured pH value, and the secondary displays shows
the temperature,

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
9. Dip the temperature probe into the solution of known temperature,
allowing some time for the temperature probe to stabilize. Press ↑↓
key to select temperature. Scroll up or down by pressing ↑↓ key to
set the correct temperature value. It allows a limit of ± 5°C variation
of the input reading and the reading originally displayed.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
10. After selecting the correct temperature, press CON to confirm.
The CON indicator flashes.
11. Press CAL/MEAS key to return to the pH measurement mode.
The temperature probe is now calibrated.

C. pH determination of a Pharmaceutical product

1. The READY mode informs that the readings are stable within a
range of ±0.01pH.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
2. To measure, rinse the electrode with distilled water before use.
This will remove impurities that have adhered on it and, will serve to
Activate.
3. Switch the meter on and ensure meter is in [MEAS] mode. This
applies whether measuring pH or mV. The MEAS annunciator is
displayed on the top center of the LCD display.
4. Dip the electrode into the sample (pharmaceutical product),
ensuring that the glass bulb of the electrode is completely immersed
into the sample. Stir the electrode gently in the sample to create
homogenous sample.
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
5. Take readings when it is stable, a READY annunciator will be
displayed. Record the readings.
6. After measuring, rinse the electrode with distilled water and store
in electrode storage bottle filter with buffer pH 4.0.
7. Measure the pH of the sample three times (three trials) with at
least 5 - minute interval.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 7. pH DETERMINATION
Questions:

1. Draw and label the parts of a typical modern pH probe or the glass
electrode.

2 Give the importance of determining the pH of pharmaceutical

products.

3. What are the uses or applications of pH measurements?

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
DELIVERABLE VOLUMEE
Deliverable volume is a test to provide the assurance that
oral liquid such as solutions, emulsions and suspensions,
when transferred from the original container or bottle, deliver
the volume that is declared on the label or label claimed
volume. This test is applicable to products labeled to contain
not more than 250mL

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 8. DELIVERABLE VOLUMEE
OBJECTIVE: To be able to perform in process testing,
deliverable volume.
APPARATUS / GLASSWARE: Graduated cylinder
MATERIALS/SAMPLES: 10 bottles of bottled
pharmaceutical liquid products (contents 10mL & 30ml)

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 8. DELIVERABLE VOLUMEE
PROCEDURE
1. Prepare the 10 bottles, shake the contents individually.
2. Gently pour the contents of each container into separate
dry graduated cylinders to avoid formation of bubbles.
NOTE:
For 10mL- use 25mL capacity graduated cylinder
For 15 mL - use 30mL capacity graduated cylinder
For 30 mL - use 50mL capacity graduated cylinder
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 8. DELIVERABLE VOLUMEE
3. Allow each container to drain for no more than 30
minutes.
4. Measure and record the volume of each bottle, make sure
it is free from air bubbles.
5. Compute the average volume of the contents of the 10
bottles.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 8. DELIVERABLE VOLUMEE
Bottle No. Label Claimed Actual Volume
Volume (ml) (ml) Computation:
DATA & RESULT: 1
2
3
Conclusion:
4
5
6
7
8
9
10
Average
Volume

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
Activity 8. DELIVERABLE VOLUMEE
Questions:
1. According to the latest USP/NF, what is the acceptance
criteria to deliverable volume?
2. In using the USP/NF acceptance criteria, what is the
disposition for the test results done in the experiment? Why?
3. What stage/s of production should deliverable volume be
performed?

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
HOMOGENEITY TEST
In process quality control (IPQC) Tests means controlling
the procedures involved in manufacturing of dosage form
from the starting materials to the distribution of the finished
products. In suspensions, one of the IPQC tests performed
is the homogeneity test using the sedimentation volume.
Sedimentation volume is defined as is the ratio between
ultimate volume of sediment to the initial volume of the
suspension. The value is between the limits 0 to 1. The
higher the sedimentation volume the better is the physical
stability
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
HOMOGENEITY TEST
OBJECTIVE: To check the homogeneity of suspension
using in-process quality control test.
APPARATUS/ GLASSWARE: 100ml graduated cylinder
MATERIALS/ SAMPLES: 10 bottles (or total volume of
300mL) of liquid product in suspension

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
HOMOGENEITY TEST
PROCEDURE
Note : Perform the sedimentation volume for suspensions
using the cylindrical graduates, as follows
1. Perform the sedimentation volume by using a 100mL
graduated cylinder.
2. Pour 100ml of the suspension into the graduated cylinder.
This serves the initial volume (Vo). Let it stand for about 3
hours.
Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021
Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
HOMOGENEITY TEST
3. After 3 hours, check the volume of the suspension.
Record this as the ultimate volume (Vu).
4. Perform three trials.
5. Compute for the sedimentation volume, using the formula.
F = Vu Where: F is the sedimentation volume
Vu is the ultimate volume
Vo Vo is the initial volume

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
HOMOGENEITY TEST
6. The sedimentation value is between the limits 0 to 1. If
the sedimentation volume is 1, no sedimentation occurred.
This means that the suspension is aesthetically pleasing, no
visible clear supernatant liquid.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
HOMOGENEITY TEST
DATA & RESULT:
Data Trial 1 Trial 2 Trial 3
Initial Volume (Vo)
Ultimate Volume (Vu)
Time started
Time Finished
Sedimentation volume (F)

Computation:

Conclusion:

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.
HOMOGENEITY TEST
QUESTIONs:
1. Give the importance of In-process Quality Control.

2 What are the other IPQC for suspension? Describe each.

Ref.Book: Jenkins Quantitative Pharmaceutical Chemistry by Knevel & Digangi, MPH@2021

Laboratory Manual in QC2 by Valencia & Gaerlan & WHO GMP Vol.2 2nd ed.