-

P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
THE UNIVERSITY OF QUEENSLAND

SCHOOL OF PHARMACY

DOSAGE FORM DESIGN A

Laboratory Manual
PHRM 2022
Semester 2 2014

Copyright 2014
School of Pharmacy, University of Queensland
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
Page
PRACTICAL SCHEDULE
GENERAL INFORMATION
EXPERIMENT 1
Powder properties
12
EXPERIMENT 2
Powder mixing
20
EXPERIMENT 3
Dissolution testing
26
EXPERIMENT 4
Tablet manufacture formulation
33
EXPERIMENT 5
Tablet manufacture granulation and compression
38
EXPERIMENT 6
Properties of solid dosage forms
42
EXPERIMENT 7
Aspirin degradation through water absorption
51
EXPERIMENT 8
Capsule Filling
59
SYNDICATES
1-5
6-10
11-15
16-20
21-25
26-30
31-35
36-40
45-48
49-52
53-56
57-60
61-65
66-70
71-75
WEEK
DATE
41-44
28 Jul
noprac noprac noprac
4 Aug
11 Aug
18 Aug
25 Aug
1 Sep
8 Sep
15 Sep
22 Sep
noprac
noprac noprac noprac noprac
MID-SEM BREAK
10
30 Sep
Public Holiday/NO PRAC
11
7 Oct
Online Calculation Test Time allocation/NO PRAC
12
14 Oct
Online Calculation Test Time allocation/NO PRAC
13
21 Oct
Competency Assessment (invitation only)

SYNDICATES 1 40:

SYNDICATES 41 80:

MORNING SESSION
9am 10.50pm
AFTERNOON SESSION 1pm 2.50pm
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
ATTENDANCE AND ASSESSMENTS

See the Electronic Course Profile (ECP) for details of attendance requirements and assessments
associated with course.
PREPARATION FOR LABORATORY CLASSES
You will get far more out of the lab sessions if you get into the habit of thoroughly reading each
experiment protocol and the background theory before arriving at the lab. You cannot expect to
perform the lab experiments efficiently if you don't know what you are supposed to be doing.
Furthermore, it is not the task of the lab demonstrators to tell you step by step what to do. They are
there to assist you to do the experiments and to help you to understand them. Organisation of your time
is important in all lab classes. You are expected to work neatly and accurately.
Bring the following items with you to every laboratory class:

Clean white laboratory coat
Closed-in footwear
Calculator
This laboratory manual
Students are required to wear a clean laboratory coat (buttoned-up, tied or zipped closed) at all times,
closed in footwear and appropriate clothing. Long hair must be tied back during laboratory sessions.
Safety glasses and gloves will be provided for you in the laboratory and must be worn if the procedure
calls for eye and/or skin protection.
The academic in charge, scientific officer or demonstrator may request a student to leave the laboratory
if shoes or clothing are considered inappropriate for Occupational Health and Safety (OH&S) reasons. In
such circumstances, the student will not receive marks for that laboratory exercise.
LOCK-OUT
Students arriving at the laboratory session later than 10 minutes following the official start of the
practical session will not be allowed to carry out the laboratory exercise and will not receive marks for
that laboratory session. For OH&S reasons, the demonstrators will detail any hazards associated with the
laboratory exercise at the start of each practical session and you must attend this to be able to work in
the laboratory.
REFERENCE TEXTS
There are no required textbooks for this course. Recommended books for reference are listed in
the Electronic Course Profile.
Official compendia and formularies are available in the laboratory and library, including:
British Pharmacopoeia (BP)

Updated annually; the library has hard copies to 2007 and online access from 2008.
Martindale The Complete Drug Reference.
The library has various editions, e.g. 2007 (35th ed)
Previously known as Martindale - The Extra Pharmacopoeia until 1996 (31st ed).
Australian Pharmaceutical Formulary and Handbook (APF)
The library has various editions, e.g. 2009 (vol 21)
United States Pharmacopeia (USP) and National Formulary (NF)
The library has various editions, e.g. 2007 (30th ed)
ASSISTANCE OUT OF CLASS TIME
Answers to your questions about academic content will usually be found in a textbook. Answers to your
questions about the structure of the course and assessments will usually be found in the ECP. Please post
questions on the Blackboard feedback forum for PHRM2022 if you are unable to find the answer in a
textbook or the ECP.
TEAMWORK
During your practicals in this and many other courses, and during your working life, you will be
operating within a teamwork environment. In the laboratory-based practicals in the School of Pharmacy
you work in a syndicate.
Individuals within a team all have unique skills and strengths. An effective team does well because of the
combined input of ALL of its members. Any individual team member can play a number of different
roles within the team. Some of the kinds of roles that people may take on are:
Leader/coordinator
Sceptic/thinker
Checker/recorder
Conciliator
Explainer
Unfortunately sometimes you may find either yourself or other team members take on roles that are
disruptive to genuine efforts to improve team effectiveness and satisfaction. For example:
being aggressive, blocking, competing or dominating

back stabbing, blaming, sarcastic or cynical
clowning or joking to disrupt the work of the group
withdrawal
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
However, be wary about blaming anybody for acting in these ways. You also need to remember that
people may interpret behaviour differently. For example, you may think someone is blocking progress
but somebody else might see it as questioning an idea; you may think someone is clowning around but
somebody else might see it as a method to diffuse tension within the group.
The key to an effective team is communication between every member. A team cannot function well if
one person dominates conversations or talks over others, or someone sits back and doesnt actively
contribute to group activities and decisions.
Some tips:
Make sure all members of your syndicate have each others contact details both email and phone
Prepare for the laboratory before arriving
Deal with problems as they arise
Dont dominate or ignore other members of the syndicate
Dont just agree with others put your perspective forward
Be an active participant you will learn more than if you let others do all the work
See the UQ student services web site for more information on making your
group work effectively:
http://www.uq.edu.au/student-services/Group+work
SAFETY RULES
1
Drugs and compounded products must not be used for self-medication, and must not
be removed from the laboratory.
2
All students must wear covered footwear during practical classes. Thongs, open weave
shoes, sandals, etc. are not appropriate footwear. Students will not be permitted to
participate in practical classes unless wearing suitable footwear.
3
A clean laboratory coat must be worn at all times whilst in the laboratory.
4
Long hair must be tied back during practical sessions. Hats, scarves and other headgear
must not be worn.
5
No eating, drinking (including drinking from water bottles) or smoking in the
laboratories.
6
Do not sit on laboratory bench tops. Sit on stools or chairs when provided.
7
Bags, coats etc., should be left in the allocated places in the laboratories.
8
Use safety glasses and/or gloves if the procedure calls for eye and/or skin protection.
9
Know the location and use of the fire-fighting appliances in and near the laboratories.
10
Know the location and use of the safety showers in the laboratories.
FIRST AID
11
12
13
14
15
REPORT ALL INJURIES to the demonstrator immediately. First aid will be

administered.
All accidents must be reported to the demonstrator and recorded online using the
Injury, Illness and Incident Reporting System (see UQ OHS website).
CHEMICAL SPILLS on skin: thoroughly wash the affected area with copious quantities
of water.
EYE INJURIES are always serious: treatment requires immediate and prolonged
flushing with water (20 minutes minimum). Medical advice should be obtained for any
eye injury.
SHARPS INJURIES: wash the wound in running water. Medical advice should be
obtained.
WASTE DISPOSAL
16
Instructions regarding disposal of all laboratory wastes must be strictly observed.
Failure to do so will result in fines being levied on the School by the University or City
Council.
17
ORGANIC SOLVENT wastes must not be discarded via the sinks due to their adverse
impact on the plumbing and the environment. Place these wastes into the marked
containers provided.
18
The YELLOW BINS are for solid waste, including paper towel. Used creams &
powders should be wrapped in newspaper before placing in the bin.
19
The SHARPS CONTAINERS located on each bench are for used pasteur pipettes, and
small pieces of broken glassware. Larger pieces should be wrapped in newspaper, taped
securely, and put in YELLOW BINS.
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
CONDUCT IN LABORATORIES
20
Students are expected to conduct themselves in a professional manner.
21
Students must not enter preparation rooms unless directed by staff.
22
Students are expected to arrive at practical sessions prepared and on time.
23
Students may not work in the laboratories outside normal class times except with
special permission from academic staff responsible for that laboratory.
24
The equipment in the laboratories is expensive, precision made and requires careful
treatment. Ask to have all equipment demonstrated before use.
HOUSEKEEPING
25
All items which are used in the course of conducting an experiment must be left in the
manner in which they were found, i.e. clean and in the appropriate place. Bench checks
will be carried out to ensure this is done.
26
DRUGS must not be removed from laboratories.
27
Return all drugs to their proper place immediately after use.
28
Keep sinks, benches and common user areas clean.
29
Clean balances immediately after use.
MULTI-USER LABORATORY RULES
30
All powders, tablets, creams, and ointments must be wrapped in newspaper, stuck
down with tape, and placed in the yellow waste bin.
PREGNANCY
31
Students who are pregnant, or are planning to become pregnant, must contact the
course coordinator before starting practical sessions. Some controls may need to be put
into place to reduce the health risks of contact with certain chemicals.
PERSONAL PROTECTIVE EQUIPMENT
32
Students must wear white lab coats and enclosed footwear to all practical sessions.
Safety glasses and gloves are provided within the laboratories and students must use
these when instructed by the demonstrator, academic or scientific staff.
The work of a pharmacist in a dispensary requires great care and attention to detail. Only
by working in a tidy and organised fashion will this be achieved. Dirty, unhygienic and
untidy work will not be acceptable in this lab, in a dispensary, or in professional practice.
Remember that the products that you prepare in your professional career are intended for
administration to a living patient -- now is the time to start learning to do things correctly.
Think carefully about everything that you do before doing it.
The definition of compounding is the preparation, mixing, assembling, packaging of a drug in the course of
professional practice. Qualified pharmacists make medications from scratch using raw materials.
Planning, workflow and hygiene
1
Plan your work area. Your workbench must be kept clean, tidy and uncluttered during work.
Bags, coats and other items not required for work are to be stored where directed by scientific
staff. Dirty spatulas and glass stirring rods should be cleaned immediately, or else placed on a
piece of clean paper, but not directly on the bench.
2
Compound liquid products by carefully considering the order of addition of components.

Where water and a cosolvent are used in the formulation, dissolve poorly-water soluble
compounds in the cosolvent. Dissolve substances with good water solubility directly in the
water, then slowly (with stirring) add the aqueous solution to the cosolvent solution. Some
aqueous solution products (e.g. those containing iodine) require that a complexing agent be
present to give the required concentration. The complexing agent MUST be dissolved in the
aqueous phase first.
Compounding Worksheets
3
All information must be recorded in a compounding worksheet, which acts as a record of
product manufacture. The compounding worksheet is retained by the pharmacy for future
reference, e.g. in the event that a patient experience an adverse reaction. Compounding
worksheets like the one over the page will be provided for you in the laboratory. See the APF
extemporaneous dispensing section for another example of a compounding worksheet.
The worksheet must be completed at the same time as compounding is performed and should
explain exactly what you do while making the product. Note that his is in contrast to a
laboratory report which is completed after you leave the laboratory and so should be written
in past tense in the style of a scientific publication. You must use ballpoint pen, not pencil.
Mistakes must be neatly crossed out and corrected, not altered using correcting fluid or
whiteout. The legal requirements for entering and correcting dispensing information in a
Dangerous Drugs register are particularly strict and require that ALL corrections be legible
and explained (Queensland Poisons Regulation, Sec H6.04).
All spaces in the worksheet must contain the appropriate information. If a category is not
appropriate to the product, write NA for not applicable. Do not leave it blank, because we
will take this to mean that you dont know the answer, have forgotten the answer, or dont
appreciate its relevance.
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
Checking procedures
6
Everyone makes mistakes: in pharmacy, development of rigorous checking procedures is
essential. All weighings and measurements must be checked by a second person and the
compounding worksheet initialled in the appropriate space.
Equipment maintenance
7
Stainless steel spatulas may react with acids, tannins, iodine, mercury salts. Sulphur is also
commonly believed to be a problem with metal spatulas as it results in discolouration. Use a
plastic or vulcanite/ebonite spatula when using substances that react or are corrosive, e.g.
salicylic acid, resorcinol.
8
Do not use an earthenware mortar and pestle with iodine. Use all glass equipment. Iodine can
enter the pores of the earthenware mortar and contaminate the next material that is put into
it.
Damp or contaminated spatulas must NOT be placed in bottles containing bulk supplies of
chemicals. Wet pipettes must not be placed in bulk liquids. Spatulas or pipettes must not be
left standing in open containers.
10
Materials spilled on or near balances must be cleaned up IMMEDIATELY.
11
Avoid spilling substances into boiling baths. Should this occur, inform your demonstrator
immediately, as the bath may need to be drained and cleaned before it can be used again.
12
Benches, sinks, slabs, balances, spatulas, measuring cylinders, etc., must be cleaned
immediately after your product is made. Residues of semi-solids must be cleaned from
mortars, pestles, basins, etc., with paper towel and then cleaning alcohol if needed (available
at sinks). Wrap semi-solid wastes in paper and place in the appropriate rubbish containers. Do
not allow dirty apparatus to accumulate on benches or in sinks or lockers.
13
Replace all lids or caps on containers after use and screw them down firmly. Make sure the
outside of each container is clean and labels are not marked by residues.
14
Use correct pouring technique (i.e., keep label uppermost) to prevent labels from becoming
contaminated and illegible.
At the end of the prac

15
Under NO circumstances are students to remove from the laboratory any student
preparations, chemicals, medications, equipment, containers, etc., unless you have explicit
permission from the academic staff member in charge.
16
Check with scientific staff before leaving the lab at the end of each class. Ensure that:
your equipment and workspace are clean and tidy
all chemicals and books have been put away
your locker has been checked and you have signed the attendance register
10
P H R M 2 0 2 2 D O S A G E F O R M D E S I G N A
The
compounding worksheet should be completed in pen (not pencil), with any mistakes crossed neatly
through (no whiteout), at the same time that the product is being prepared.
Name of
person/
people/
syndicate
preparing
the product
Date of
preparation
Name of product
Name of each ingredient in

the formulation
Schedule for each
ingredient, if scheduled in
the SUSMP (name change
from SUSDP from July
2010)
Actual
weight or
volume
measured
Batch number
and expiry as
indicated on
the container
If the formula specified an

ingredient in terms of % and you
have to calculate the weight/vol
then show % here
Initials of the
person that
checked the
accuracy of the
entries for each
ingredient
e.g. APF21, Mater Hospital formulary, prescription
The method should reflect exactly what was done to compound the product.
For example:
Weighed out the ingredients

Crushed the tablet and mixed with the other
powders using geometric progression in a pestle
and mortar
Storage and expiry information: Use standard conditions for the type of
formulation (see APF) unless the formulation specifies otherwise
Notes may include any warning labels or instructions given to the patient, e.g.
shake the bottle, external use only
11
INTRODUCTION
This experiment is designed to show you some basic properties of powders:
(1)
(2)
(3)
(4)
Density
Porosity
Flow properties
Cohesiveness
DENSITY
Density is generally defined as weight (mass) per unit volume. Three density definitions are of
importance for powders:
(a)
(b)
(c)
True density is the density of the solid material alone and is the mass of the solid per true
volume of the solid (exclusive of pores within the particles and void spaces between the
particles). True density is determined by gas displacement, or by very high pressure
compaction.
Bulk density is the total volume of the solid, pores and void space between the particles which
is calculated as the mass of the solid divided by the bulk volume, both of which are easily
measured with general lab weighing and measuring apparatus.
Granule density is the mass of the solid divided by the granule volume i.e. the total volume of
the solid and pores within the particles. The granule volume is measured by displacement of a
liquid such as mercury, which has a high surface tension and cannot enter the pores.
Table 2.1. Comparison of bulk density (g/cm3) with true density measured by a helium displacement
or granule density measured by liquid displacement.
Bulk Density True Density Granule density
Bismuth Subcarbonate, Heavy
1.01
6.9
Bismuth subcarbonate, Light
0.22
6.9
Magnesium Carbonate, Heavy
0.39
3.0
Magnesium Carbonate, Light
0.07
3.0
Phenobarbital
0.34
1.3
Sulfathiazole
0.33
1.5
Talc
0.48
2.7
12
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
Table 2.2. True density (g/cm3) of solids used in Pharmacy

Aluminium Oxide
4.0
Mercuric Chloride
Benzoic Acid
1.3
Mercuric Iodide
Bismuth Subcarbonate
6.86
Mercuric Oxide
Bismuth Subnitrate
4.9
Mercurous Chloride
Bromoform
2.9
Paraffin
Calcium Carbonate (Calcite)
2.72
Potassium Bromide
Calcium Oxide
3.3
Potassium Carbonate
Chalk
1.8-2.6
Potassium Chloride
Charcoal (air free)
2.1-2.3
Potassium Iodide
Clay
1.8-2.6
Sand, fine dry
Cork
0.24
Silver Iodide
Cotton
1.47
Silver Nitrate
Gamboge
1.2
Sodium Borate, borax
Gelatin
1.27
Sodium Bromide
Glass Beads
2.5
Sodium Chloride
Graphite
2.3-2.7
Sucrose
Kaolin
2.2-2.5
Sulfadiazine
Magnesium Carbonate
3.04
Sulfur, Precipitated
Magnesium Oxide
3.65
Talc
Magnesium Sulfate
1.68
Zinc Oxide (hexagonal)
5.44
6.3
11.1
7.15
0.90
2.75
2.29
1.98
3.13
1.5
5.67
4.35
1.73
3.2
2.16
1.6
1.50
2.0
2.6-2.8
5.59
POROSITY
When powders are packed in a container, the total void volume relates to the space within and between
the particles.
v = Vb - Vp
where v
Vb
Vp
= void volume
= bulk volume
= true volume of particles
Total porosity () is defined as the ratio of the void volume to the bulk volume, i.e.:
= v/Vb = (Vb - Vp )/ Vb
Porosity is usually expressed as a percentage.
13
FLOW PROPERTIES
Deformation of a powder occurs on the application of a force causing relative displacement of mass
without moving the centre of gravity. If the application of the force causes continuous deformation with
time and involves movement of the centre of gravity of the particles, the powder is said to flow. The
"flow properties" of a powder reflect this ability of particles to flow and powder may be classified as
free-flowing or sticky. The ability of powders to flow is of importance in many areas of pharmaceutical
processing, including tableting, capsule filling, mixing, bulk transfer and packaging. Factors influencing
flow properties include:
particle size and distribution

particle shape
surface texture
moisture content
particle density
Cohesive powders are interactive, and are not free-flowing. The particles in a cohesive powder bind
with each other forming agglomerates and aggregates. These types of powders will interact with other
powders forming discrete ordered units or will interact with equipment causing difficulty in processing.
The forces involved in these interactions are electrostatic, capillary and chemical.
The angle of repose () is one method to measure powder flow. The angle of repose is defined as the
maximum angle between the surface of a pile of powder and the horizontal plane.
The angle of repose is calculated from:
tan = height(h)/radius(r)
= tan-1 (h/r)
14
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
EXERCISE 1.1
DENSITY and POROSITY
OVERVIEW
You will determine the bulk density and porosity for three powders:
unlubricated tablet granules (true density 1.5 g/ml)
heavy magnesium carbonate (true density 3.0 g/ml)
light magnesium carbonate (true density 3.0 g/ml)
NOTE: Keep all equipment dry do not wash equipment after use.
NOTE: Keep the three powders separate they will be re-used by the next class.
METHOD
1.
2.
3.
4.
Sieve a sample of about 50 mL of powder through a number 20 sieve.

Put the sieved powder into a pre-weighed 100 mL cylinder and weigh the filled cylinder in order to
calculate the mass of powder.
Drop the cylinder on the bench surface three times from a height of 25 mm at 2 second intervals.
Note the volume this is the bulk volume.
Return the powders to their containers.
RESULTS
Record the mass of powder and bulk volume to 3 significant figures. Use the data to calculate the bulk
density and total porosity of each powder.
EXERCISE 1.2
FLOW PROPERTIES: ANGLE OF REPOSE
OVERVIEW
You will investigate powder flow by measuring the angle of repose for three powders containing different
particle diameters:
<250 m
250-425 m
>425 m
NOTE: Keep the three powders separate they will be re-used by the next class.
METHOD
Each member of the syndicate should perform the following method once for each powder, resulting in
either 3 or 4 replicate measurements of the angle of repose for each powder.
1. With the cylinder placed on top of the sample table provided, fill the cylinder with powder to the
appropriate level, then lift it clear of the powder. The excess powder will flow off the edge of the
sample table.
2. Measure the height of the powder mound and record your results.
3. Return the powders to their containers.
15
RESULTS
Present a table containing powder height and use the data to calculate angle of repose for each replicate
measurement. Calculate the mean and standard deviation angle of repose for each powder.
EXERCISE 1.3
FLOW PROPERTIES: COHESIVENESS
OVERVIEW
You will investigate powder flow by measuring cohesiveness of three powders containing different
granules (A or B or C) by mixing small quantities of B or C with a large quantity of A and observe their
interaction using the microscope.
METHOD
1. Mix 1 g of A with 100 mg of C in the jar provided for 60 sec.
2. Observe the mix using the microscope by placing a small sample of the mix on the glass slide. Note
any associations between particles if present. Draw one field of view.
3. Place the remainder of the mix on the nest of sieves provided (425m, 180 m, pan). Combine
your powder with the powders from other groups before sieving in a sieve shaker for 5 minutes (see
your demonstrator). Observe the content of each sieve.
4. Repeat the process using 1 g of A and 100 mg of B.
5. Dispose of the mixed powders.
RESULTS
Briefly explain your observations of cohesiveness using your drawings of the field of view and the
particle sizes observed after sieving.
ASSESSMENT
Assessment of your syndicates performance in this laboratory is based on the data sheets that you
complete. An example of the data sheet is included below. All members of your syndicate will receive the
same mark.

16
P H R M
2 0 2 2
D O S A G E
EXPERIMENT 1.1
F O R M
D E S I G N
SYNDICATE NUMBER:
Results: Density and porosity of three contrasting powders

Powder
unlubricated tablet
heavy magnesium
light magnesium
granules
carbonate
carbonate

Mass of powder (g)

Bulk volume (ml)

Bulk density (g/ml)

True density (g/ml)

True volume (ml)

Total porosity (%)

What is the difference between heavy and light magnesium carbonate that leads to the
differences in total porosity?

What would you expect to happen to total porosity if the polydispersity of particle size is
increased?

How do you think increasing particle density will affect powder flow?

How do you think increasing porosity will affect powder flow?

17
EXPERIMENT 1.2
SYNDICATE NUMBER:
Results: Angle of repose for three contrasting powders

Particle diameter:
<250 m
250-425 m

Student 1 Height

Angle of repose

Student 2 Height

Angle of repose

Student 3 Height

Angle of repose

Student 4 Height

Angle of repose

Average
Angle of repose

Std dev
Angle of repose

Based on your results, how does increasing particle size affect powder flow?

18

>425 m
P H R M
2 0 2 2
D O S A G E

EXPERIMENT 1.3
F O R M
D E S I G N
SYNDICATE NUMBER:
Results: Angle of repose for three contrasting powders

Mixture: 1000 mg A + 100 mg C
Mixture: 1000 mg A + 100 mg B

Observed cohesiveness
Observed cohesiveness

Particle sizes determined by sieving
Particle sizes determined by sieving

Based on your results, how does particle size affect powder flow?

Tutor use only
Table 1.1 correct, and 3 sig fig
Table 1.1 questions answered correctly
Table 1.2 correct
Table 1.2 question answered correctly
Table 1.3 as expected
Table 1.3 question answered correctly
Complete
2
2
2
1
2
1
Small
errors
1
1
1
0.5
1
0.5
Major
errors
0
0
0
0
0
0
Tutor initials

19
INTRODUCTION
Powder mixing is very important in pharmacy, because dose uniformity for dispensed or proprietary
solid dosage forms depends on the even dispersion of small quantities of potent drugs in one or more
inert solid diluents called excipients.
Forces involved in mixing or demixing (segregation) a multi-particulate solid system:
forces that tend to move adjacent particles, or groups of particles, relative to each other
(i) translational and rotational forces
(ii) centrifugal forces
(iii) gravitational forces
forces that hold adjacent particles, or groups of particles, in a fixed position

(i) electrostatic cohesive force
(ii) capillary cohesive force
(iii) molecular cohesive force
Mixing mechanisms are generally characterized as follows:

1) convective mixing which is the bulk transfer of solids around the mixer. This transfer can be
caused by rotation of mixers, use of paddles or agitators and directional change in mixer
rotation.
2) shear mixing caused by movement of adjacent planes of particles in the mixer system.
3) diffusive mixing which occurs by random diffusion of dissimilar particles in the powder mix.
Factors affecting the mixing process include:
particle sizes
proportion of active substance to inactive excipients
tendency of powders to aggregate
mixing mechanism (and therefore forces) applied
time of processing to allow a truly random condition to be achieved
prevention of segregation when the mixing operation ceases
Powder mixers are classified as:

a) Tumbling mixers: A simple cylindrical drum revolving about its axis results in powder movement
mostly within one plane. Improvement by ensuring convective mixing is achieved by the
incorporation of baffles or helical flights or by modification of the mixer design, eg cubes
mixer, double cone mixer, V-shell blender.
20
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
b) Agitation mixers rely on shear forces produced by physical means such as mechanical devices or
by air blasts. The shear forces can be localised so improvement by ensuring convective
movement is required.
EXPERIMENT 2
COMPARISON OF METHODS FOR POWDER MIXING
OVERVIEW
In this experiment you will use four different methods to mix two powders together, two methods that
involve tumbling and two that involve agitation. You will then measure the success of your mixing
technique by measuring dose uniformity. The powders have different particle sizes and colours so that
you can see visually as well as spectrophotometrically how well you have mixed them together.
PRE-LAB PREPARATION
These questions are to be completed prior to proceeding with the laboratory experiments, and your
answers will be checked by the tutor because it is important that you comprehend what you are
expecting to measure before you start.
If copper carbonate and heavy magnesium carbonate are mixed in a ratio of 1:4
a. How much of each of the powders are required to make 25 g total?
b. What is the concentration (%) of copper carbonate in this mixture?
c. If powder mixing is perfect, how much copper carbonate would you have in 500 mg?
d. If you dissolve 500 mg of the mixed powders in 50 mL, and powder mixing was perfect,
what is the expected concentration of copper carbonate in mg/100 mL?
PROCEDURE
1. Powder mixing
Weigh out the appropriate quantities of copper carbonate and heavy magnesium carbonate to create a
number of 25 g mixtures in the ratio 1:4. Then mix the powders using the four techniques available.
The number of samples to be prepared, and the mixing techniques to be used are shown in Table 2.1.
Table 2.1 Four methods of powder mixing
Powder mixing method
Type of mixing method
Number of mixes
Erweka Cube Mixer, 10 minutes
tumbling mixer, in 3 planes
One 25 g mixture per syndicate

All syndicates combined for mixing
Rolling Cylinder, 10 minutes
tumbling mixer, in 1 plane
Mortar and pestle, 10 minutes
geometric progression
One 25 g mixture per student
Spatulation on a slab, 10 minutes
geometric progression
21
2. Visual assessment of mixing

Make a visual assessment of powder mixing for each method based on observations of powder colour.
3. Spectrophotometric assessment of mixing
Measure the concentration of copper carbonate in the required samples (see Table 2.2) using the
following method:
(a)
Transfer samples of approximately 0.5 g (write down the weight used) into dry 50 mL
volumetric flasks.
(b)
Carefully and slowly (in small amounts) add 10% sulphuric acid to each flask and make up to
volume. Sulphuric acid is corrosive, can burn you and is harmful by inhalation be careful.
(c)
Measure the absorbance of the solution on the spectrophotometer at 810 nm, using a 1 cm
plastic cuvette and 10% sulphuric acid as the reference solution (also known as the blank).
Table 2.2 Samples to be analysed

Number of mixes
Number of samples analysed
Erweka Cube Mixer

All syndicates combined for mixing
1 sample per syndicate,

collect results from 2 other syndicates
Rolling Cylinder
3 samples per syndicate
Mortar and pestle
Spatulation
4. Clean up
All flasks must be washed out first with dilute sulphuric acid, then distilled water, then placed in the
plastic boxes provided (not back in the cupboard).
WARNING!
10% SULFURIC ACID is harmful by inhalation. Causes burns. Risk of serious damage to eyes. WEAR
GOGGLES. To clean contaminated surfaces, use water. Flush eyes with running water for at least 15
minutes and seek medical attention.
22
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
RESULTS
1. Write down the concentration of copper carbonate in mg/100 mL.
Standard Curve Copper Carbonate

0.8
y = 0.9503x - 0.0063
Absorbance (810 nm)
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
-0.1
0.2
0.4
0.6
0.8
Copper Carbonate (g/100ml)
2. Calculate the concentration of copper carbonate in mg/g of sample, and calculate the mean and
standard deviation for the 3 replicate samples from each mixing technique.
ASSESSMENT
Assessment of your syndicates performance in this laboratory is based on the data sheets that you
complete. All members of your syndicate will receive the same mark.

23
EXPERIMENT 2
SYNDICATE NUMBER:
Results: Mixes created using four contrasting mixing techniques

Sample
Weight
CuCO3
CuCO3

analysed (mg) (mg/100 mL)
(mg/g)

rep 1

Erweka
Cube mixer
rep 2

rep 3
rep 1
rep 2
rep 3

rep 1
Mortar and
pestle
rep 2
rep 3

rep 1
Spatulation
rep 2
rep 3

Rolling
cylinder
24

mean

std dev
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
Rank your mixing methods based only on visual assessment of mixing.

What should the concentration of CuCO3 (mg/g) be if the powders were perfectly mixed?

Explain which mixing method is most accurate based on your results.

Explain which method is most reproducible based on your results.

Tutor use only
Table correct, calculations correct
Appropriate sig figs used
Correct expected conc of CuCO3
Correct interpretation of results
Complete
5
2
1
2
Small
errors
2.5
1
0.5
1
Major
errors
0
0
0
0
Tutor initials

25
INTRODUCTION
Solid dosage forms do not dissolve in solvents such as water and body fluids instantly, but require
appreciable time for the dissolution process. The dissolution rate of a drug is an important factor in
determining its bioavailability and its onset of action. A drug with low aqueous solubility is likely to have
a slow dissolution rate, a low or erratic oral bioavailability and a slow onset of action. The dissolution
rate (rate of solution) of solids was first described by Noyes and Whitney, using:
dc
= k (Cs Ct )
dt
Concentration
where dc/dt is the dissolution rate, i.e. the amount of drug, dc (in mg), dissolved in the medium in the
time interval dt (sec), k is a constant, Cs is the saturated solubility of the drug in the medium (mg/L)
and Ct is the concentration dissolved (mg/L) at any time t after the introduction of the drug into the
solvent. A typical dissolution profile is shown in Fig. 4.1.
Time
Fig. 4.1: Plot of drug concentration (Ct) as a function of sampling time (t)
Later, it was shown that the constant, k, was made up of three terms:
k=
DA
h
where D (cm2/sec) is the diffusion coefficient of the drug (related to the speed at which the drug moves
through the medium), S (cm2) is the total surface area of the drug particles and h is the thickness (cm) of
the diffusion layer around the drug particles.
26
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
The diffusion layer is a layer of water molecules which are immobilized by adhesive forces with the solid
particles. This layer is also called the unstirred or stagnant layer. Its thickness is variable and hard to
define, but is typically 0.005 cm (50 m) or less and is affected by stirring of the medium or agitation.
The terms in the Noyes-Whitney equation affect the dissolution rate in different ways:
increase in S gives increased dissolution rate
increase in D gives increased dissolution rate
increase in Cs gives increased dissolution rate
increase in Ct gives decreased dissolution rate
increase in h gives decreased dissolution rate
Other factors also alter dissolution rates:
increased temperature increases both Cs and D
ionisation of the drug (to a more polar species) by a change in pH will increase Cs
The decrease in rate shown by the curvature of the plot in Fig. 4.1 results from either a decrease in A
(as some particles especially smaller ones dissolve and surface area of larger particles decreases as the
particles slowly dissolve), or an increase in Ct (approaching Cs and thereby reducing the magnitude of
the term Cs-Ct), or commonly both. The early linear region depicted in the plot is observed if the
decrease in A over the initial time period is not significant and if sink conditions prevail ie the difference
between Cs and Ct remains constant. It is conventional to assume that sink conditions are maintained if
Ct is less than 10% of Cs.
The dissolution test is defined by the USP and BP. Usually a large beaker (1 L) is used, with carefully
defined dimensions, in a controlled temperature water bath (37C). The contents of the beaker are
stirred by a paddle or other device which rotates at a controlled rate. The solvent, normally either
simulated gastric fluid (SGF) or simulated intestinal fluid (SIF,) is placed in the beaker and allowed to
equilibrate to the desired temperature, then the weighed sample is added (time = 0). Samples are taken
regularly, using a filter to prevent any particles of undissolved drug being taken (which would give
falsely high results). The samples are then assayed for the drug concentration. The concentration is
plotted as a function of time (see Fig. 4.1).
The Noyes-Whitney equation is not the only way of quantifying dissolution rates. It can be shown for
uniformly sized particles that the Hixson-Crowell cube root law describes the dissolution rate in terms
of the amount undissolved, Mt, at any time, t:
13
13
M
M
= t
o
t
where Mo is the initial weight of drug particles, Mt is the weight undissolved at time t, and is a
constant. This equation predicts that a plot of Mo1/3 - Mt1/3 as a function of time is a straight line with
slope and an intercept of zero. If the plot is not linear, or the intercept 0, then the initial assumption
that the particles are all the same size cannot be correct. Unlike the Noyes-Whitney equation, the
prediction of linearity of the plot is not affected by the dissolution of the particles, and hence by changes
in particle size or solution concentration.
27
EXPERIMENT 3
OVERVIEW
The aim of this experiment is to investigate the effects of pH on the dissolution rate.
You are provided with paracetamol powder. Paracetamol is a weak acid which ionises in water (pKa
9.5). You will use a standard dissolution test apparatus and method which complies with the United
States Pharmacopoeia (USP). The dissolution will be examined at both an acidic pH (SGF) and a basic
pH (pH 9.5).
NHCOCH3
NHCOCH3
+ H 3O +
+ H2O
OH
O-
METHODS
Each syndicate will use 2 beakers for the dissolution test. One beaker contains 900 mL of Simulated
Gastric Fluid (SGF) which is pH1.5 and contains sodium chloride and hydrochloric acid, the other
contains sodium hydroxide and sodium chloride at pH 9.5. The water bath in which the beakers sit is
maintained at 37C, and the stirring speed is 50 rpm.
Dissolution test
1.
Weigh the following (record the weight accurately):

2 x 100 mg of paracetamol (>250 m).
2.
Place the paracetamol in the SGF and start the stopwatch.

Remove 5 mL samples at 1, 2, 4, 6, 10, 15, 20, and 30 minutes after the start.
Replace each 5 mL sample with 5 mL of fresh SGF.
3.
Approximately 5 minutes after the start of the previous test, start the experiment with the
paracetamol in pH9.5, sampling at 1, 2, 4, 6, 10, 15, 20 and 30 minutes after the start.
Analysis of paracetamol concentration in samples

Dilute 2 mL of each sample to 50 mL with SGF and determine the absorbance at 244 nm.
28
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
RESULTS
Record your results. Determine the concentration using the calibration curve provided below.
Absorbance at 244 nm
0.8
0.7
y = 1.336x
0.6
0.5
0.4
0.3
0.2
0.1
0
0
0.05
0.1
0.15
0.2
0.25
0.3
0.35
0.4
0.45
0.5
Paracetamol concentralon (mg/50 mL)
Using the data that you have calculated, plot a graph that shows the total amount of paracetamol that is
dissolved with time and estimate the time that it took for 50% of the paracetamol to be dissolved.
ASSESSMENT
Assessment of your syndicates performance in this laboratory is based on the data worksheets that you
complete. Example worksheets are shown below. You will be provided with worksheets and graph paper.
All members of your syndicate will receive the same mark.
29

EXPERIMENT 3
SYNDICATE NUMBER:
Results: Dissolution of paracetamol in SGF

Time i
ii
iii
(min) Absorbance Concentration Amount
(mg/50 mL)
dissolved in

the 900 mL

dissolution

media (mg)

iv
Amount
dissolved in
the 5 mL
sample
retrieved
(mg)

Time taken for 50% of the paracetamol to dissolve in SGF:

30
v
Total amount
dissolved
(mg)
(=iii+sum of iv up
to previous
sample)

P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N

Results: Dissolution of paracetamol pH 9.5
Time i
ii
iii
(min) Absorbance Concentration Amount
(mg/50 mL)
dissolved in
the 900 mL
dissolution
media (mg)

iv
Amount
dissolved in
the 5 mL
sample
retrieved
(mg)

v
Total amount
dissolved
(mg)
(=iii+sum of iv up
to previous
sample)
Time taken for 50% of the paracetamol to dissolve in SGF:

31
1. Explain the difference in the two plots for the different pHs

2. Would you expect to see any difference in dissolution profile for paracetamol if the
dissolution test was performed using a different particle size at pH 9.5? Explain your answer.

Tutor use only
Tables correct, calculations correct
Correct graph of total amount vs time with labelled axes
and title
Appropriate estimates of time to 50% dissolution
Correct answer to Qu 1
Correct answer to Qu 2
32
Complete
4
2
Small
errors
2
1
Major
errors
0
0
Tutor initials

1
1
2
0.5
0.5
1
0
0
0
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
This experiment is in two sections which are essentially independent. This

experiment involves the basic formulation of a tablet ingredients into a mucilage.
Experiment 4. includes the process of granulation and tablet compression.
INTRODUCTION
In this experiment you will
manufacture granules by the moist granulation process.
follow the requirements of the Code of Good Manufacturing Practice during production.
Phenobarbitone tablets B.P. are uncoated tablets for oral use. They are prepared by the moist
granulation process using starch mucilage as the binder. The granules are then compressed into tablets
using a Rotary Punch Tablet Press. The tablets should conform to B.P. specifications.
The formulation for phenobarbitone tablets B.P. is:
Phenobarbitone
Starch
Lactose
Starch mucilage (10% w/w)
Magnesium stearate
125 mg
30 mg
30 mg
qs
0.75%
PROCEDURE
1.
You are required to manufacture these tablets using the "Manufacturing Formula" provided.
The Manufacturing Formula contains the tablet specifications, formulation, detailed method of
manufacture and packaging and label requirements.
2.
Calculate quantities for a batch size of 500 tablets.
3.
The Control number should be as follows:

P(phenobarbitone) - (surname initials of group) - (date in the form DDMMYY)
eg. P-ABCD-081010
ASSESSMENT
Assessment of your syndicates performance in this laboratory is based on the manufacturing formula and
33
answers to questions that you complete. Example worksheets are shown. You will be provided with the
manufacturing formula and worksheets in the lab. All members of your syndicate will receive the same
mark.
EXPERIMENT 4
SYNDICATE NUMBER:
MANUFACTURING FORMULA
Product: PHENOBARBITONE TABLETS B.P. 125 mg
Formula written by:
Formula checked by:
Mr B Hughes
Dr P Cabot
Date:
Date:
Production authorised by:
Control Number:
Batch Size:
500
SPECIFICATIONS
Theoretical
Identification
Actual
Notes
B.P. Tests
Assay
1. Phenobarbitone
92.5 107.5 %
2.
3.
Uniformity of content
NA
Weight (target)
190 mg approx.
Uniformity of weight
BP:
Tablets in the range
80-250 mg must be
7.5%
Disintegration time
30 minutes (max.)
Dissolution rate
NA
Hardness
5 2 kg
Thickness
NA
Friability
< 1 % loss in 10
min.
Colour
white
Other
NA
Actual weight depends on the

amount of starch mucilage
used.
PACKAGE AND LABEL

Type of container
Size
Method of packaging
Remarks
34
Affix complete label here.
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
Packaged by
Date
Amount
per unit
Processing step, ingredient and directions
Control number:
Batch size: 500 tablets
Raw
material
control no.
Initials
Amount per
batch
weigher checker
MIXING
125 mg
1. Weigh required mass of phenobarbitone

into an empty stainless steel bowl.
2. If the powder is lumpy, screen through 20
mesh sieve into the final bowl with the help
of a stiff nylon brush.
30 mg
3. Weigh required mass of starch into an

empty stainless steel bowl.
30 mg
5. Weigh required mass of lactose into an

empty stainless steel bowl.
7. Blend the phenobarbitone, starch and
lactose in the Erweka Agitation Mixer for 5
minutes.
MUCILAGE MANUFACTURE
8. Boil about 120 g distilled water in a 250
mL beaker using a hotplate
15 g
9. Weigh starch into a pre-weighed 250 mL

beaker.
45 g
10. Weigh COLD distilled water into the

same beaker. Disperse the starch in the
water using a glass stirring rod.
11. Weigh 90 g of the boiling water to the
dispersed starch in the beaker.
12. Place the beaker on a hotplate and stir
until the starch has gelled, i.e. allow bubbles
to rise through the mixture for about 2 mins
DO NOT CHAR THE STARCH.
13. Allow to cool by taking off the hotplate
35

Amount
per unit
Control number:
Raw
material
control no.
Initials
Amount per
batch
weigher checker
KNEADING/MIXING
14. Add the starch mucilage in SMALL
portions to the mixed powders in a stainless
steel bowl. Knead by hand until the powder
mass becomes slightly moist, but not sticky.
When consistency is right (similar to dry
scones), reweigh the beaker and the
remaining starch mucilage.
Weight of beaker + remaining mucilage
= ___________________________ g
Weight of washed and dried beaker
= ___________________________ g
Weight of starch mucilage used in batch
= ___________________________ g
15. Shape mass into 3 or 4 fist-sized balls.
MOIST (WET) GRANULATION
16. Granulate the mass using the Erweka
Moist Granulator, using a perforated disc.
DRYING
17. Dry the moist granules in the Hot Air
Suspension Dryer for 15 min. Set inlet
temperature to 60C and the outlet
temperature should be close to 40C.
After 10 minutes break the crust that forms
on the surface of the granules.
After ~ 20 mins the temperature will be the
same at the outlet as the inlet, which is when
the drying is finished.
36
Weight of
starch used in
batch =
________ g
Total batch
weight =
________ g
P H R M
2 0 2 2
D O S A G E
EXPERIMENT 4
F O R M
D E S I G N
SYNDICATE NUMBER:
A. What is the function of each component of the tablet formulation?

B. Show the calculation of the theoretical weight of the tablet

Tutor use only
Manufacturing formula completed; weigher/checker initials
Correct answers to Qu A
Correct answers to Qu B
Complete
5
2
3
Small
errors
2.5
1
1.5
Major
errors
0
0
0
Tutor initials

37

INTRODUCTION
This experiment is in two sections which are essentially independent. This
experimental process (5) involves the granulation of the dried mucilage and tablet
components into granules and then compression to a tablet form. Experiment 4.
involves the basic formulation of a tablet ingredients into a mucilage.
In this experiment you will

manufacture granules by the moist granulation process from either 5 or a supplied granule
sample.
compress Phenobarbitone tablets B.P. 125 mg using the Manesty Rotary Punch Tablet Press.
follow the requirements of the Code of Good Manufacturing Practice during production.
Phenobarbitone tablets B.P. are uncoated tablets for oral use. They are prepared by the moist
granulation process using starch mucilage as the binder. The granules are then compressed into tablets
using a Rotary Punch Tablet Press. The tablets should conform to B.P. specifications.

38
P H R M
2 0 2 2
D O S A G E
EXPERIMENT 5
F O R M
D E S I G N
SYNDICATE NUMBER:

Amount
per unit
Control number:
Raw
material
control no.
Initials
Amount
per batch
weigher checker
MILLING
18. Set up the Erweka Oscillating Granulator
with a size 20 mesh screen in place.
19. Pass the dry, oversize granules through the
oscillating granulator to produce dry granules >
20#.
20. Weigh out a 100 g sample of the granules
(allows for easy discussion in terms of %).
21. Gently shake these granules on a 60 mesh
sieve for 15 20 seconds onto a large sheet of
weighing paper.
(do not overdo because will create more fines)
22. Weigh the fines that pass through the 60#
screen.
Weight = ________________________ g
23. Determine the percentage of fines in the
entire batch.______________________ %
24. Weigh the batch of granules.
Weight = ________________________ g
25. Weigh an excess amount of magnesium
stearate and sieve through a 80# sieve.
0.75 %
26. Weigh enough sieved magnesium stearate

to lubricate the batch.
27. Mix the magnesium stearate with the
granules in the Erweka Agitation Mixer for 5
min.
COMPRESSION
28. Using 8 mm punches and dies, set up the
four stations on the Manesty Rotary Punch
Tablet Machine Model B3B.
29. Adjust the weight screw to give a tablet
weight of ____________________ mg.
30. Adjust the compression screw to give a
hardness of ___________________ kg.
39
31. Compress the granules and monitor the

tablet weight to produce
(
g) for 10 tablets
and a tablet hardness of
(
kg) for the batch.

Discard the first few tablets because the dies
are warming up so size changes.
Check the weight of 10 tablets to ensure the
weight is correct and adjust machine using the
weight adjustment screw if needed
Once tablet weight is correct, then adjust the
punches if hardness is not in range.
32. Dedust the compressed tablets by shaking
briefly over a 10# screen.
33. Weigh the final batch of tablets and
calculate the yield
= ________________________ %
34. Package in quarantine container until
quality control releases batch run for
consumer packaging.
40
P H R M
2 0 2 2
D O S A G E
EXPERIMENT 5
F O R M
D E S I G N
SYNDICATE NUMBER:
C. What is the significance of calculating the percentage of fines?

D. Show the calculation of % yield

E. Summarise the main steps in tablet manufacture in granulation and compression.

Tutor use only
Manufacturing formula completed; weigher/checker initials
Correct answer to Qu C
Correct answer to Qu D
Correct answer to Qu D
Complete
5
2
2
1
Small
errors
2.5
1
1
0.5
Major
errors
0
0
0
0
Tutor initials

41
PRE-LAB PREPARATION
It is essential that you find the appropriate BP tests and requirements that are used in this prac before
you come to the lab. Copies of the BP will be available in the lab, but if you are unprepared and have to
search the BP for the information during the prac it is unlikely that you will finish all of the tasks.
You should also check the questions and calculations on the worksheets and make sure that you know
the answer or how to calculate the answer.
The BP is not easy to search! Take some time to look through the book or the online copy accessible
through the UQ library. The sections you will require are listed below. Once you have found these
sections you need to work out what the BP tells you to do for each experiment in this practical.
Volume III - Formulated Preparations: General Monographs
Tablets
Volume III - Formulated Preparations: Specific Monographs
Aspirin Tablets
Dispersible Aspirin Tablets
Effervescent Aspirin Tablets
Gastro-resistant Aspirin Tablets
Volume IV Appendices
Consistency of formulated preparations
Disintegration
Friability
Resistance to Crushing of Tablets
INTRODUCTION
Tablets and capsules should possess a number of desired attributes.
(a)
(b)
(c)
(d)
(e)
42
Ability to withstand the rigors of mechanical treatment involved in production, packaging,

distribution and dispensing.
Free from defects such as specks, discolouration, chips, or contamination.
Uniformity in weight and drug/excipient content.
Chemical and physical stability during storage and use.
Ability to release the drug in a reproducible and predictable manner.
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
In order to ensure solid dosage forms with the required properties, manufacturers employ a number of standard tests, some
of which are specified in the British Pharmacopoeia (BP). The BP tests are usually the same as those in the European
Pharmacopoeia (Ph Eur). For example, the BP has standard operating procedures for the following tests:
Identification of active ingredient

Content of active ingredient
Uniformity of content
Uniformity of diameter for tablets
Uniformity of weight
Disintegration
Dissolution
Resistance to crushing of tablets
Friability
Note that tablets either pass or fail the test; they do not pass well or only just pass the test.
AIMS
In this series of experiments you will compare three different forms of aspirin tablets using BP tests.
Fig. 6.1. structure of aspirin

The BP defines different types of tablets in the section Tablets (Volume III - Formulated Preparations: General
Monographs).
The tablet types that you will compare are:
Tablet type
Effervescent
Dispersible
Immediate release
Gastro-resistant
Coated/uncoated
Uncoated
Uncoated
Uncoated
Coated
Brand
Aspro Clear
Solprin
Aspro
Cartia
BP tests that you will undertake are:

1. Uniformity of weight (do this test first and re-use the tablets for the other tests)
2. Identification
3. Resistance to crushing
4. Friability
5. Disintegration
43
EXERCISE 6.1
UNIFORMITY OF WEIGHT
The weight of a tablet produced in any manufacturing procedure is proportional to the volume of the
die fill. Because there may be variations in this volume caused by factors such as the flow properties of
the granules and differences in the bulk density of the same granule batch, the weights of the tablets
produced will not be exactly the same. The BP gives the % deviation allowed.
METHOD
The BP specifies that a uniformity of weight test is required for all uncoated tablets in the section Tablets
(Volume III - Formulated Preparations: General Monographs).
Find the uniformity of weight test in the BP: Volume IV Appendix XII C. Consistency of Formulated
Preparations.
Perform the BP uniformity of weight test for the uncoated tablets:
Effervescent tablets (Aspro Clear)
Dispersible tablets (Solprin)
Immediate release tablets (Aspro)
RESULTS
*** Reuse these tablets in the other tests ***
Tabulate the weights and calculate the mean. What are the BP specifications for uniformity of weight for
tablets? Do the tablets pass or fail the BP test for uniformity of weight?
EXERCISE 6.2
IDENTIFICATION
The active component of the tablets must be identified in the raw materials before manufacture and
again for the final product before distribution. The identification tests are shown in the individual
monographs in the BP and European Pharmacopoeia.
METHOD
1. Perform the BP identification test for Immediate and Dispersible Aspirin Tablets (Solprin). This is
the test that identifies the presence of aspirin. (Note: no heating required, tutor will guide on
immediate release identification process before starting)
2. Read the BP identification test for Gastro-resistant Aspirin Tablets (Cartia). You will not perform
these tests today due to the strong chemicals involved.
The methods are given in the Specific Monograph for each dosage form in Volume III of the BP.
RESULTS
Tabulate your results. Do the tablets pass or fail the BP test? Explain the reaction involved in the test
and the result obtained.
44
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
EXERCISE 6.3
RESISTANCE TO CRUSHING
Manufacturers need to check tablet hardness or mechanical strength, which may influence tablet
disintegration and dissolution.
METHOD
Find the Resistance to Crushing of Tablets test in Volume IV, Appendix XVII of the BP.The method involves
using an automated Hardness Tester which has units of measurement in Newtons.
Perform the BP resistance to crushing test for the uncoated tablets:
RESULTS
Present the results as instructed by the BP Resistance to Crushing of Tablets.
EXERCISE 6.4
FRIABILITY
Manufacturers need to test the ability of tablets to withstand abrasion due to normal handling and
transporting conditions.
METHOD
Find the Friability test in Volume IV, Appendix XVII of the BP.The method involves using an automated
Wear and Tear Tester and is only used for compressed uncoated tablets.
Perform the BP friability test for the uncoated tablets:
RESULTS
Calculate the percentage of material lost for each group of tablets. Do the tablets pass or fail the BP test
for friability?
45
EXERCISE 6.4
DISINTEGRATION
The European and British Pharmacopoeia specify that tablets must conform to certain disintegration
requirements (see Tablets: Volume III - Formulated Preparations: General Monographs). Each type of tablet
has its own disintegration test.
These tests ensure that the tablets will break down to smaller particles in the gastrointestinal tract,
allowing dissolution of the active ingredient and absorption.
METHOD
Perform the BP Disintegration test for each of the four types of tablet:
Immediate release tablets (Aspro) use the standard test for uncoated tablets
Gastro-resistant tablets (Cartia) this will be performed as a single batch by the demonstrator
The tests are described in the BP section Tablets which is in Volume III - Formulated Preparations: General
Monographs.
RESULTS
Record the disintegration time for each tablet tested. Do the tablets pass the relevant BP test?
ASSESSMENT
complete. Example worksheets are shown. You will be provided with worksheets in the lab. All members
of your syndicate will receive the same mark.
46
P H R M
2 0 2 2
D O S A G E
EXPERIMENT 6
F O R M
D E S I G N
SYNDICATE NUMBER:
6.1 Results of the BP Uniformity of Weight test

Effervescent
Dispersible

Tablet weights

Mean

% dev allowed
according to BP

Minimum tablet
weight allowed

Maximum tablet
weight allowed

Result: Pass/Fail

Immediate release

47

6.2 Results of the BP Identification test

Immediate

Average tablet weight

Weight of aspirin per tablet

Weight of powdered tablet
equivalent to 50 mg aspirin

Colour reaction result

Result: Pass/Fail

Explain the reaction involved
in the test and so why it works
for aspirin

48
Dispersable

P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
6.3 Results of the BP Resistance to Crushing test

Effervescent
Dispersible
Force applied to

crush tablets

Mean

Minimum

Maximum

6.4 Results of the BP Friability test

Effervescent
Dispersible
Average tablet

weight

Number of tablets

used for testing

Total weight of

tablets before test

Total weight of

tablets after test

% material lost

% material loss

allowed according
to BP
Pass/fail

Immediate release

Immediate release

49

6.5 Results of the BP Disintegration test

Medium used for
test (e.g. water)

Max time allowed
for disintegration
according to BP

Observed
disintegration
times

Pass/fail

Effervescent

Dispersible

Immediate release

Gastro-resistant

acid
pH6.8
Tutor use only

6.1 Uniformity of Weight
6.2 Identification
6.3 Resistance to crushing
6.4 Friability
6.5 Disintegration
50
Correct
Small errors
Incorrect/incomplete
2
2
2
2
2
1
1
1
1
1
0
0
0
0
0
Tutor
initials

P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
PRE-LAB PREPARATION
It is essential that you find the appropriate BP tests that are used in this prac before you come to the lab.
Copies of the BP will be available in the lab, but if you are unprepared and have to search the BP for the
information during the prac it is unlikely that you will finish all of the tasks.
You should also check the questions and calculations on the worksheets and make sure that you know
the answer or how to calculate the answer.
In this prac, you will need the following sections of the BP:
Volume I&II Monographs: Medicinal and Pharmaceutical Substances Salicylic acid
Volume III Formulated Preparations: General Monographs Tablets
Volume IV Appendix XVII Resistance to Crushing of Tablets
INTRODUCTION
The adsorption of gases onto solids can be characterised by various adsorption isotherms. Water
adsorption on solids is classified by type II and type III isotherms in the Brunauer classification (Fig. 6.1).
Fig. 7.1. Isotherms for the adsorption of water onto solids.

The type II isotherm is indicative of a strong physical adsorption showing monolayer adsorption
followed by multi-layer adsorption. Type III is typical of weak interaction between the water adsorbate
and the solid surface showing no distinct segment of monolayer adsorption.
51
The adsorption of water onto solid surfaces can be modelled using the treatment of Brunauer, Emmett
and Teller (BET equation):
(C 1) P
P
1
=
+
V(PO P) VMC VMC PO
where v is the volume of water vapour adsorbed at pressure p, po is the saturated vapour pressure of
water, vm is the volume of water adsorbed to provide monolayer surface saturation and C is a constant
which equals:
(E1 E L )
C = k.exp
RT
where k is a constant related to the net entropy of adsorption, E1 is the heat of adsorption of the first
layer, EL is the heat of liquification of water and is assumed to represent the heat of adsorption for the
multilayers. The BET equation parameters (Vm and C) can be obtained from a linear plot of p/v(po-p)
versus p/po.
Whether a type II or a type III adsorption isotherm occurs for particular systems depends on the relative
heats of adsorption for monolayer and multilayer water adsorption.
Both type II and type III isotherms have been observed for drugs, pharmaceutical excipients and solid
dosage forms. Many of the common tabletting excipients, including sugars, starch, methylcellulose and
ethylcellulose exhibit type III isotherms; magnesium trisilicate and zimelidine dihydrochloride show
type II behaviour. However, not all powders absorb water (Table 6.1).
TABLE 7.1 Some powders that do not absorb or desorb water
Sulphathiazole
Phenobarbitone
Benzocaine
Talc
Quinine
Niacin
Phenothazine
Diphenylhydantoin
Chloramphenicol
Codeine
Prochlorperazine maleate
Aminophylline
Water associated with solids can be considered bound or unbound. Bound water physically interacts
with the solid and possesses an equilibrium vapour pressure less than pure water since it:
(a) may contain dissolved solids in high concentration,
(b) may be trapped in fine capillary pores or
(c) may be molecularly bound as a hydrate within the solid.
Unbound water possesses an equilibrium vapour pressure equal to pure water and condenses at a
relative humidity of 100%. Under most conditions encountered in processing or storage of
pharmaceutical powders, adsorbed water will be bound.
Water adsorbed onto a solid interacts physically with that solid, producing the characteristic type II and
III isotherms. However, water can be molecularly bound within solids in the formation of crystalline
hydrates. In such cases, characteristic isotherms unlike any of the Brunauer classification exist.
52
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
The adsorption or desorption of water associated with solid powders presents several potentially severe
stability problems.
(a)
Promotion of chemical degradation

Adsorbed water can promote surface chemical degradation of drugs susceptible to decomposition
reactions. The mechanism of degradation involves dissolution of the drug in the adsorbed moisture
film, followed by chemical decomposition of the saturated drug solution. Aspirin in the solid state
hydrolyses by this mechanism with zero order kinetics. Degraded aspirin tablets will possess a
characteristic acetic acid odour. They will become yellow, due to the formation of a ferric
salicylate complex from the presence of minute traces of iron. Adsorbed water has also been
shown to influence the degradation of aminosalicylate and ascorbic acid.
Adsorbed moisture can destroy effervescent solid dosage forms. The water causes release of
carbon dioxide from the tablet or powder, due to premature reaction between tartaric or citric
acid and alkaline substances such as sodium bicarbonate or calcium carbonate in the formulation.
The moist appearance of such dosage forms (due to both adsorbed moisture and water which may
be produced during reaction) is characteristic of this type of degradation, and is due to improper
packaging or storage conditions.
(b)
Loss of integrity of gelatin capsules

Hard gelatin capsules consist of gelatin, plasticizers and water with optional components such as
preservatives, colouring and opacifying agents. The capsules have a moisture content between 12
and 15%. Storage in high humidity conditions, with resultant moisture content rising above 16%,
causes the capsules to become sticky, distorted, lose mechanical strength and cause problems
during automated filling procedures. Conversely, desorption of moisture to below about 10%
causes shrinkage and brittleness, and they become susceptible to breaking and cracking on
mechanical stress.
Soft gelatin (or flexible) capsules consist of gelatin and water, with glycerol, sorbitol or propylene
glycol as a plasticizer and may contain colouring agents, preservatives and opacifying agents.
Physical stability is also concerned with adsorption or desorption of moisture from the capsule
shell. Generally, conditions which cause desorption of water, i.e. relative humidity <20% or high
temperatures (>40C) cause brittleness with subsequent greater susceptibility to mechanical
shock. However, these effects are transient and soft gelatin capsules stored under normal humidity
conditions will return to normal. High humidity conditions (>60%) provide irreversible damage
causing the capsules to become softer, tackier and bloated.
(c)
Changes in solid dosage form properties

The adsorption or desorption of water can produce marked changes in solid dosage form
properties. Changes in tablet hardness, disintegration, weight and dissolution characteristics have
been reported with gain and/or loss of moisture. This form of physical degradation may modify
the properties to such an extent that the dosage form is no longer effective, i.e., tablets become so
soft that they crumble or dissolution changes might cause poor bioavailability. Excipients such as
sucrose, dextrose, sorbitol, mannitol and lactose all showed marked decreases in tablet hardness
with increase in the storage relative humidity e.g. storage at 75% RH caused a decrease from 15
(Strong Cobb units) to 1.2 (equivalent to 10.6 kg down to 1 kg) after only two days for a sucrosebased tablet.
53
Degradation caused by adsorption of water can be minimized by proper control of the manufacturing
process and by selection of packaging materials. The stability of a pharmaceutical product must always
be fully tested in the final packaging before release to the distribution warehouse. In addition, the
pharmacist must store materials appropriately and must instruct patients on storage. Physical
degradation will most often occur when drugs are stored incorrectly, i.e., tablets and capsules taken out
of foil or blister packs, bottles stored with caps removed, or else stored in high humidity environments
(especially in the bathroom).
EXPERIMENT 7
OVERVIEW
In this experiment you will study the degradation of aspirin in an effervescent aspirin tablet (Aspro
Clear) stored at different relative humidity conditions over a four week period.
Fig. 7.2. The ester bond in aspirin hydrolyses in the presence of water
Aspro Clear, removed from their strip packaging, have been stored at 22.5% and 59% relative humidity
(RH) 4 weeks. Tablets which have stored in their foil strip at room RH are the experimental control.
Each syndicate will have 12 tablets from each of the five storage treatments on which to carry out
the following tests:
7.1.
7.2.
7.3.
7.4.
7.5.
Tablet appearance. The tablets are then to be used in other determinations.

Tablet weight. The tablets are then to be used in other determinations.
Salicylic acid content for 3 of the tablets (i.e., extent of chemical degradation).
Hardness for 3 of the tablets (i.e., extent of physical degradation).
Disintegration time for 6 of the tablets (i.e., extent of physical degradation).
ASSESSMENT
complete. Example worksheets are shown. You will be provided with worksheets in the lab. All members
of your syndicate will receive the same mark.
54
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
EXERCISE 7.1
APPEARANCE
A subjective comment regarding the appearance of the tablets should be made. Note any colour
changes, mottling, dampness of the tablet, etc.
EXERCISE 7.2
AVERAGE TABLET WEIGHT
Determine the average tablet weight by weighing all 12 tablets at once and calculating the weight of one
tablet.
Determine the percent change in tablet weight for each group of tablets (i.e. the difference storage in
foil vs removed from strip packaging expressed as a %).
EXERCISE 7.3
SALICYLIC ACID CONTENT
To assess the chemical degradation of the aspirin to salicylic acid we can either measure the decline in
concentration of aspirin or the increase in concentration of salicylic acid.
The BP Assay for salicylic acid in the monograph for Salicylic acid in Monographs: Medicinal and
Pharmaceutical Substances, BP Volume I&II involves titration of salicylic acid with sodium hydroxide, with
an indicator to show visually when the sodium hydroxide has neutralized the salicylic acid. We cannot
use this method because aspirin is also an acid, so the test is not able to differentiate between the two
compounds.
Instead we will perform an assay for salicylic acid that is based on UV spectroscopy.
Procedure:
Powder 3 tablets in a glass mortar and take a quantity of powder equivalent to 300 mg of aspirin. Dilute
appropriately with the buffer (pH 7) provided.
N.B. The appropriate dilution will depend on the degree of degradation. Initially, or where little
decomposition is suspected, try a dilution to 100 mL; where marked degradation has taken place,
further dilution may be required.
Measure the absorbance of each solution at 298.5 nm with a 1 cm quartz cell.
Use the calibration curve equation (Fig. 7.3) to calculate the concentration of salicylic acid in your
tablets. Remember to account for the different dilutions that you may have applied to each type of
tablet.
Calculate also the % degradation that has taken place (i.e. reduction of aspirin content as a % of the
original level).
55
1.2
y = 0.3125x
Absorbance
1
0.8
0.6
0.4
0.2
0
0
0.5
1.5
2.5
3.5
Concentralon (mg/100mL)
Figure 7.3. Calibration plot for the absorbance at 298.5 nm against concentration of
salicylic acid (mg/100 mL)
EXERCISE 7.4
RESISTANCE TO CRUSHING
Find the Resistance to Crushing of Tablets test in Volume IV, Appendix XVII of the BP.The method involves
using an automated Hardness Tester which has units of measurement in Newtons.
To save time, perform the test for 3 tablets instead of 10. Present your results as required by the BP
test.
EXERCISE 7.5
DISINTEGRATION TIME
Perform the BP disintegration test for effervescent aspirin tablets. The test differs for each type of
tablet, so find the correct one in the BP section Tablets which is in Volume III - Formulated Preparations:
General Monographs.
Also, give subjective comments on the quality of the effervescence (e.g. strong, moderate or wimpy
fizzer) and determine whether the tablets pass or fail the BP test for disintegration.

56
P H R M
2 0 2 2
D O S A G E
EXPERIMENT 7
F O R M
D E S I G N
SYNDICATE NUMBER:
7.1 Tablet appearance after storage treatments

Treatment
Tablet appearance

Control (foil strip)

59% RH, 4 weeks

7.2 Average tablet weight after storage treatments
Treatment
Weight of 12 tablets Average tablet weight % change in weight

0%

59% RH, 4 weeks

7.3 Salicylic acid content after storage treatments
Treatment
Weight of
Absorbance
Salicylic acid
Aspirin
powdered
at 298.5 nm
content
degradation
tablet used
(mg/tablet)
(%)
(mg)


59% RH, 4 weeks

7.4 Resistance to crushing after storage treatments
Treatment
Force
mean
minimum
maximum


59% RH, 4 weeks

57
7.5 Disintegration after storage treatments

Treatment
Observed
Max time
Descriptive
disintegration
allowed for
assessment of
times (min)
disintegration
quality of
according to
effervescence
BP


59% RH, 4 weeks

Tutor use only
7.1 Appearance
7.2 Average weight
7.3 salicylic acid content
7.4 Resistance to crushing
7.5 Disintegration
58
Correct
Small errors
Incorrect/incomplete
1
2
3
2
2
0.5
1
1.5
1
1
0
0
0
0
0
Pass/fail
Tutor
initials

P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
PRE-LAB PREPARATION
1. If a child weighing 10 kg is prescribed 15 mg/kg q6h prn, what dose of paracetamol is given?
2. The pharmacist dispenses 10 capsules containing the oral powder. In the process of making the
capsules the pharmacist measured a displacement value of 1.4 for paracetamol with respect to
lactose. How much lactose (mg) is equivalent to the paracetamol dose (mg) in question 1 when
measured in terms of volume?
3. If 600mg of lactose fills one 00 capsule, how much lactose would be contained in the capsule with
the paracetamol dose calculated in question 1? (hint allow for displacement)
INTRODUCTION
Powders are defined in APF20 as ...mixtures of two or more powdered medicaments intended for oral
administration, though powders for external use may also be prepared. Divided (or single dose) powders
of potent actives for internal use are not commonly prepared extemporaneously but there are still
circumstances when they may be required, e.g. when a suitable divided dose is not available commercially,
there is no documented liquid formulation, or there is a lack of stability/efficacy data for making a liquid
dosage form. In this practical we will look at compound powders prepared into capsule dosage forms.
Inert diluents (usually lactose) are added:
1. if the quantity of the active is less than approximately 100 mg for capsules; for ease of handling the
minimum weight of a powder should be 200 mg
2. for transparent capsules, because the capsules look better if relatively full
Advantages of using oral powders:
more stable than a liquid formulation
administration can be relatively easy
faster absorption than solid dosage forms such as tablets
Disadvantages of using oral powders:
potential for dose variation due to incomplete mixing
potential for wrong dose due to incorrect calculation by pharmacist
bulky and inconvenient to carry
59
General method for preparing capsules

There are two ways to fill capsules:
1) by weight
2) by volume
Handle capsules as little as possible to avoid contamination with grease and moisture either use spare
capsule halves as holders or wear gloves.
Table 3.3. Capsule sizes and approximate capacities (mg) according to Winfield & Richards (2004)
Capsule number:
000
00
0
1
2
3
4
5
Capacity (mg)
950
650
450
300
250
200
150
100
1) Capsule filling by weight
Essentially this approach describes an individual dose that is weighed out is placed into a capsule. Can be
time-consuming if many capsules have to be filled.
a) Select a suitable capsule size reference texts give approximate sizes but these can vary due to
differences in bulk density or filling method. If unsure simply fill a capsule and see what weight of
powder you are able to fit in. For aesthetics, choose a total volume that will safely fit inside your
chosen capsule and will look reasonably full.
b) Calculate the required amount of diluents and medication to fill one capsule
c) Calculate the total amount of diluents and medication required to make an excess of the number of
capsules (e.g. make 12 capsules if 10 are required)
d) Weigh the total amount of each component
e) Mix the powders using geometric progression
f) Weigh out the individual powder from the mix and pour into a capsule. This can be done with the
aid of a folded piece of weighing paper, or with paper folded to make a funnel.
2) Capsule filling by volume
a) Select a suitable capsule size
b) Calculate the required amount of each diluent and medication to fill one capsule
The volume taken up by 1 g of a powder varies due to differences in bulk density (see prac 1). A
medication with a low bulk density will take up more space and therefore displace more of the diluent
than the same weight of a powder with a high bulk density. When filling by volume (such as a capsule,
or a pessary or suppository mould), bulk density must be taken into account. The displacement factor
of an ingredient is defined as the number of parts by weight of the ingredient that displaces one part
of the diluent.
i. For each powder, fill a tared capsule (larger half), tap on the bench to remove unfilled spaces,
and weigh the contents. Do this in triplicate & take the average.
ii. Calculate the displacement factor work out how much medication would displace 1 g of
diluent.
iii. Calculate the required amount of diluent & medication to fill one capsule.
iv. Calculate the amount of both components to make an excess of the number of capsules required
(e.g. make 12 capsules if 10 are required)
c) Weigh the total amount of each component
d) Mix the powders using geometric progression
e) Fill the capsules in a consistent manner, tapping on the bench to remove unfilled spaces. It is good
practice to check the weight of your filled capsules to ensure that your filling method is consistent.
60
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
References for compounding with powders:

Ansel HC. Pharmaceutical Calculations (Any Edn.). Lippincott, Williams & Wilkins
Langley C, Belcher D (2008) Powders and capsules. In FastTrack Pharmaceutical Compounding and
Dispensing, Pharmaceutical Press, UK. p.151-165.
Marriott JF, Wilson KA, Langley CA, Belcher D (2010). Powders and capsules. In Pharmaceutical
Compounding and Dispensing 2nd Edn, Pharmaceutical Press, UK. p.195-205.
Rees JA, Smith I, Smith B (2005) Density, displacement volumes and displacement values. In
Introduction to Pharmaceutical Calculations, Pharmaceutical Press, UK. p. 125-146.
Winfield AJ, Richards RME (2004) Powders and granules. In Pharmaceutical Practice, 3rd Ed. Churchill
Livingstone, UK. p225-234.
61
EXPERIMENT 8
COMPOUNDING POWDERS
AIMS
This exercise is designed to provide practice at the required calculations, preparation and packaging for oral
powders. The prescription below is for a child who cannot take the commercially available paracetamol
liquid dosage forms.
PROCEDURE
1) Prepare the products according to the prescriptions. The doctor has given the paracetamol dose in
mg/kg, so ask the parent (your demonstrator) for the weight of your patient in order to calculate the
dose and therefore calculate what you will prepare.
2) For the purposes of this exercise each syndicate should make both A) and B):
A) 10 capsules filled by volume.
B) 10 capsules filled by weight.
Lactose should be used as the diluent. Each student should fill one capsule, as well as ensure they
understand the calculation methods.
3) Plan your method carefully
Weight/volume of each component
Who will measure, who will check
Equipment required to make the product
Order of component addition
Point of transfer to the final container
Do not proceed with compounding until your calculations have been checked.
Use the compounding worksheets available in the lab for recording all aspects of the preparation.
Prepare the medicine and label with consideration to the final aesthetics of the preparation. After the
product has been checked and marked by the tutor, attach the label to the worksheet. These are to be
handed in to the tutor prior to advancing to the analysis section below.
ASSAY for PARACETAMOL
Use the spectrophotometer available for the determination of the concentration of Paracetamol in each
of 3 selected capsules randomly selected from you pool of 10 for A) and B).
PROCEDURE
1) Transfer the whole contents of each of 3 randomly selected capsules from A) and from B) to
separate 100ml Volumetric flasks. Make up the flasks accurately to 100ml with 0.1 M NaOH.
62
P H R M
2 0 2 2
D O S A G E
F O R M
D E S I G N
2) Further dilute the samples by 1:200 to achieve an absorbance in the middle of the standard curve
displayed below
3) Blank the spectrophotometer with 0.1 M NaOH at 257 nM (ask tutor for assistance and be cautious
with sodium hydroxide as its very corrosive).
4) Concentration can be determined accurately from a spectrophotometric analysis curve for A=ecl which
is displayed as the line equation on the standard curve below:
Paracetamol Std Curve
y = 686.89x + 0.0055
R = 0.99964
Absorbance (257 nM)
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0
0.0002
0.0004
0.0006
0.0008
0.001
0.0012
Concentradon (g/100ml)
63
EXPERIMENT 8
SYNDICATE NUMBER:
Sample
Abs. at max
Conc.
paracetamol
in cuvette
(%)

A1
A2
A3
B1
B2
B3
Conc. paracetamol in the

undiluted solution (%)
Weight of paracetamol
in capsules (mg)
Average weight of paracetamol in capsules by weight (mg)

Average weight of paracetamol in capsules by volume (mg)

Tutor use only
DURING THE PRAC
Compounding worksheet for capsules is

correct
10 capsules that are acceptable to be
dispensed
Label for the capsules is correct
Dose by weight method is accurate (~5%)
Dose by volume method is accurate (~5%)

64
Correct Small Incorrect/incomplete Tutor

errors
initials

2
1
0

2
2
2
2
1
1
1
0
0
0
P H R M
2 0 2 2
D O S A G E
5/7/2010
F O R M
D E S I G N
5/7/2010
ASSESSMENT
Assessment of your syndicates performance in this laboratory is based on the compounding worksheets
that you complete, products that you make and the accuracy in your dosage form preparation. You will be
provided with compounding worksheets. All members of your syndicate will receive the same mark.
POST-LAB REFLECTION
If you were presented with a prescription for a capsule that you had to prepare while on duty in a
pharmacy, would you be confident enough to prepare the product? Think back over the method you
used and be sure that you understand why each step was performed in the way that it was only when
you understand what you are doing will you be able to perform the task competently in the future.

65

-

Încărcat de

Informații document

Drepturi de autor

Formate disponibile

Partajați acest document

Partajați sau inserați document

Opțiuni de partajare

Vi se pare util acest document?

Este necorespunzător acest conținut?

Drepturi de autor:

Formate disponibile

-

Încărcat de

Drepturi de autor:

Formate disponibile

P H R M

THE UNIVERSITY OF QUEENSLAND

DOSAGE FORM DESIGN A

noprac noprac noprac

noprac noprac noprac noprac

Public Holiday/NO PRAC

Online Calculation Test Time allocation/NO PRAC

Online Calculation Test Time allocation/NO PRAC

Competency Assessment (invitation only)

AFTERNOON SESSION 1pm 2.50pm

ATTENDANCE AND ASSESSMENTS

Bring the following items with you to every laboratory class:

British Pharmacopoeia (BP)

being aggressive, blocking, competing or dominating

REPORT ALL INJURIES to the demonstrator immediately. First aid will be

Compound liquid products by carefully considering the order of addition of components.

Materials spilled on or near balances must be cleaned up IMMEDIATELY.

At the end of the prac

Name of each ingredient in

If the formula specified an

e.g. APF21, Mater Hospital formulary, prescription

Weighed out the ingredients

Table 2.2. True density (g/cm3) of solids used in Pharmacy

particle size and distribution

DENSITY and POROSITY

Sieve a sample of about 50 mL of powder through a number 20 sieve.

FLOW PROPERTIES: ANGLE OF REPOSE

FLOW PROPERTIES: COHESIVENESS

Results: Density and porosity of three contrasting powders

Results: Angle of repose for three contrasting powders

Results: Angle of repose for three contrasting powders

forces that hold adjacent particles, or groups of particles, in a fixed position

Mixing mechanisms are generally characterized as follows:

Powder mixers are classified as:

Type of mixing method

Erweka Cube Mixer, 10 minutes

tumbling mixer, in 3 planes

One 25 g mixture per syndicate

Rolling Cylinder, 10 minutes

tumbling mixer, in 1 plane

One 25 g mixture per syndicate

Mortar and pestle, 10 minutes

One 25 g mixture per student

Spatulation on a slab, 10 minutes

One 25 g mixture per student

2. Visual assessment of mixing

Table 2.2 Samples to be analysed

Number of samples analysed

Erweka Cube Mixer

One 25 g mixture per syndicate

1 sample per syndicate,

One 25 g mixture per syndicate

3 samples per syndicate

Mortar and pestle

One 25 g mixture per student

3 samples per syndicate

One 25 g mixture per student

3 samples per syndicate

Standard Curve Copper Carbonate

Absorbance (810 nm)

Copper Carbonate (g/100ml)

Results: Mixes created using four contrasting mixing techniques

Rank your mixing methods based only on visual assessment of mixing.

Weigh the following (record the weight accurately):

* Reuse these tablets in the other tests *