Professional Documents
Culture Documents
2 Friability test
4 Disintegration test
5 Spectrometry:
UV-vis
6 Dissolution test
7 Refractometry
8 ph Determination
9 Rotatory power:
Polarimetry
10 Chromatography
Name:____________________________________
Section:__________________________________
Year/semester:____________________________
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Activity no. 1
Weight Variation
Objectives:
To be able to demonstrate the skills and technique of accuracy and precision in preparing linear
graphs as presentation of data.
Materials:
20 pcs of capsules
20 pcs of tablets
Forceps
Graphing paper
Calculator
Analytical balance
Watch glass
A. Procedure :
1. Weight each tablet in an analytical balance, record the weight of each of the tablet.
a. average weight
b. % weigh variation
c. standard deviation
d. relative standard deviation
e.relative average deviation
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B. Procedure
2. Plot a graph using your data; determine the UCL and the LCL .
C. Procedure
1. Represent and make a graph of your data on a graphing paper.
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Laboratory activity Assessment:
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Activity no. 2
Friability Test
Objectives:
To be able to know the principles behind Friability testing.
To perform Friability testing on tablets.
To perform basic calculations prior to Friability test
Discussion:
Friability is the tendency for a tablet to chip, crumble or break following compression. This
tendency is normally confined to uncoated tablets and surfaces during handling or subsequent
storage.
It can be caused by a number of factors including poor tablet design (too sharp edges), low
moisture content, insufficient binder, etc.
For obvious reasons, tablets need to be hard enough such that they do not break up in the
bottle but friable enough that they disintegrate in the gastrointestinal tract.
Based on an original design by Roche, the friability tester has now become an accepted
standard throughout the pharmaceutical industry for determining the resistance of uncoated
tablets to the abrasion and shock experienced in manufacturing, packing and shipping
operations.
Whilst the basic design remains unchanged, considerable advances have been made in terms
of reliability and ease of usage which have now been incorporated into current units
Tablets are constantly subjected to mechanical shocks and aberration during the manufacturing,
packing and transportation process.
Such stress can lead to capping, aberration or eve breakages of the tablets.
In order to monitor the resistance of tablets to such stress and to decide on their suitability for
further processing such as coating, tablets are routinely subjected to friability tests.
Friability is defined as the % of weight loss by tablets due to mechanical action during the test.
Tablets are weighing before and after testing and friability are expressed as a percentage loss
on pretest tablet weight.
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Friability is closely related to tablet hardness and is designed to evaluate the ability of the tablet
to withstand aberration in packing, handling and shipping.
INSTRUMENTATION:
Friabilator
Makes use of a tumbling apparatus where tablets are exposed to rolling and repeated
shocks from free fall within the apparatus.
SPECIFICATIONS:
There should not be any damaged or broken tablet.Not More Than 1% loss in weight.
Calculations:
initial weight
Materials: 10 -20 generic tablets and 10-20 branded tablets of the same active constituent.
Procedure:
1. Connect the socket and AC power supply source with attached power cord.
2. Turn on the switch the indicator light initializes the tester for 10mins.
3. The first status is the reset position, revolution is auto set to 100R the speed of rotation
is 25rpm.
4. Weight the tablets
5. Put the rotational part off the level axis and lock the bolts. Press start button then the test
process begins.
6. After 100R rotating at 25rpm the rotation part stops to measure the samples friability.
7. Turn off; the indicator indicates off status then the tester stops.
8. Remove the tablets from the tumbler
9. Weight the samples again.
10. Calculate % weight loss.
11. Repeat using branded tablets
12. Compare generic to brand as to % weight loss
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Data GENERIC TABLET Branded TABLET
Name: Name:
initial weight
final weight
% weight loss
CALCULATIONS:
CONCLUSIONS:
Name:___________________________________________ Date:_______________________
Group:___________________________________________
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1. Based on the United States Pharmacopeia what are the Physical tests applicable to
tablet formulation? List and describe each.
2. What are the Official tests and Non-official tests for solid dosage forms such as
tablets? List and describe each.
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Laboratory activity Assessment:
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Activity no. 3
Objectives:
To be able to know the principles behind hardness testing for tablets
To perform Hardness test on tablets.
To perform basic calculations prior to Hardness test
Discussions:
The Tablet’s ability to resist the chipping, abrasions, pulverizations, or breakages under the
conditions of storage, handling, shipping and transportation is called hardness or crushing
strength.
The extent or depth of one surface to another surface of a tablet refers to its thickness.
Instrumentation:
Most of the tablet hardness testers are hand held and operated manually. The Tablet is
placed between two flat plates. A pressure is applied until the tablet fractures or breaks
off.
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Tablet thickness
Materials:
8 chewable tablets
8 ordinary tablets
8 sublingual tablets
Venier caliper
a. Put tablet in end cone head of the tester then rotate hand wheel and exert pressure
slowly, move it forward. In time, the instrument will indicate pressure, Max of pressure 1
reader of the pressure exerted to break tablet into pieces.
b. Make four trials and take the average of the three tablets.
a. Inspect four tablets; you may use a clean brush or tissue paper if any debris is observed.
b. Used forceps to hold tablet in place, measure the thickness using the venier caliper.
c. Record your reading and compute for the average.
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HARDNESS TEST
THICKNESS TEST
COMPUTATIONS:
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Name:___________________________________________ Date:_______________________
Group:___________________________________________
1. Search for any new type model of hardness tablet tester in any reference and resources,
place the picture and description in the space provided.
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2. Interpret the following Venier Caliper readings:
a. b.
c. d.
e. f.
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Laboratory activity Assessment:
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Activity no. 4
Disintegration Test
Objectives:
To be able to know the principles behind disintegration testing.
To perform comparativedisintegration testing between generic and branded tablets.
Discussion:
This test is provided to determine whether tablets or capsules disintegrate within the prescribed
time when placed in a liquid medium under the experimental conditions presented below.
For the purposes of this test disintegration does not imply complete dissolution of the unit or
even of its active constituent.
Complete disintegration is defined as that state in which any residue of the unit, except
fragments of insoluble coating or capsule shell, remaining on the screen of the test
apparatus or adhering to the lower surface of the discs, if used, is a soft mass having no
palpably firm core.
INSTRUMENTATION:
Disintegration apparatus
General specifications:
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Apparatus A
Use apparatus A for tablets and capsules that are not greater than 18 mm.
• a basket-rack assembly
• 138–160 mm in height and having an inside diameter of 97–115 mm for the immersion
fluid
• a device for raising and lowering the basket in the immersion fluid at a constant
frequency rate between 29 and 32 cycles per minute, through a distance of not less than
53 mm and not more than 57 mm.
Place one dosage unit in each of the six tubes of the basket and if specified add a disc.
Operate the apparatus using water as the immersion fluid unless another liquid is
specified and maintain its temperature at 35–39 °C.
At the end of the specified time lift the basket from the fluid and observe the dosage
units: all of the dosage units have disintegrated completely.
If one or two dosage units fail to disintegrate repeat the test on 12 additional dosage
units.
The requirements of the test are met if not less than 16 of the 18 dosage units tested are
disintegrated
Apparatus B
• The main part of the apparatus is a rigid basket-rack assembly supporting 3 cylindrical
transparent tubes 77.5 ± 2.5 mm long, 33.0 mm ± 0.5 mm in internal diameter and with a
wall thickness of 2.5 ± 0.5 mm.
• Each tube is provided with a cylindrical disc 31.4 ± 0.13 mm in diameter and 15.3 ± 0.15
mm thick, made of transparent plastic with a relative density of 1.18–1.20. Each disc is
pierced by 7 holes, each 3.15 ± 0.1 mm in diameter, 1 in the center and the other 6
spaced equally on a circle of radius 4.2 mm from the center of the disc.
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• The tubes are held vertically by 2 separate and superimposed rigid plastic plates 97 mm
in diameter and 9 mm thick with 3 holes
In each of the 3 tubes place 1 tablet or capsule and, if prescribed, add a disc; suspend
the assembly in the beaker containing the specified liquid.
Operate the apparatus using water as the immersion fluid unless another liquid is
specified for the prescribed period, withdraw the assembly and examine the state of the
tablets or capsules.
To pass the test all 6 of the tablets or capsules must have disintegrated.
Disintegration Media
2. a. Distilled water
Materials:
Specifications:
Procedures:
Refer to the procedures presented depending on what type of apparatus will be used.
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DATA:
DATA:
Remarks/conclusion:
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Name:___________________________________________ Date:_______________________
Group:___________________________________________
1. Compare the difference between USP method and BP method for disintegration test for
enteric coated tablets.
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2. Search for the diagram of Apparatus A and B for disintegration test. Paste them in the
space provided and label accordingly.
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Laboratory activity Assessment:
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Activity no. 5
Objectives:
Discussion:
• Frequency is the number of wave cycles that travel past a fixed point per unit of
time, and is usually given in cycles per second, or hertz (Hz).
Instrumentation:
Spectrometer UV-VIS
Procedure:
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1. Turn on the power supply, allow time to warm up for about 15 to 30 mins.
2. First set up the wavelength by pressing NM. Enter the wavelength where your
measurement will be based then press set NM.
3. For Blank cell holder, place the blank or measure blank button, the machine will start its
initial reading then it will return to standby mode.
4. Take the blank cell holder then placed the cuvette containing the sample into chamber
5. Allow the machine to read and wait to stabilize.
6. After reading wash the cuvette with clean distilled water and set to dry.
7. Turn the machine off.
Data:
Conclusions:
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Name:___________________________________________ Date:_______________________
Group:___________________________________________
1. Illustrate the basic parts of a Spectrometer, label and explain each part and its function.
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2. What are the uses of UV-Vis Spectrometer?
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Laboratory activity Assessment:
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Activity no. 6
Dissolution Test
Objectives:
To be able to learn the principles of Dissolution test and its application to pharmaceutical
quantitative analysis.
To learn the basic parts of a Dissolution tester, its function and operation.
Discussion:
Dissolution is the process through which a solute gets dissolved into a solvent and forms a
solution.
Solubility is a quantitative term defining the maximum amount of solute which gets dissolved
into the solvent.
Tablet Dissolution
is a standardized method for measuring the rate of drug release from a dosage form. The
principle function of the dissolution test may be summarized as follows:
Instrumentation;
Materials
Thermometer
Pipette
Volumetric flask
Rubber aspirator
Mefenamic generic 500mg
Mefenamic Branded 500mg
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Procedure:
1. This experiment will be performed by the whole class. Each interval will be assigned by
the instructor. All data must be recorded accordingly.
2. Place dosage form in the basket in an upright position.
3. Submerged into the media, monitor and maintain the temperature at 37 degrees
centigrade.
4. Push the drive head to the vertical operating position selected put the cover and switch
on.
5. Take samples at a 15min. interval, using syringe or pipette. Withdraw an aliquot of 1ml.
6. Transfer this volume to a 100ml volumetric flask; add distilled water to make volume.
7. Take a portion and determine its absorbance using the spectrometer.
8. Repeat the procedure using the sample.
Data:
Sample (Generic)
Reference (Branded)
Spectral reading
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Computation:
Conclusions:
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Name:___________________________________________ Date:_______________________
Group:___________________________________________
1. What are the different types of Dissolution apparatus? Give each of their description. List
their advantages and disadvantages.
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Laboratory activity Assessment:
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Activity no. 7
Refractometry
Objectives:
To be able to learn and apply the principles behind the science of refractometry.
To be able to learn the basic parts, functions and applications of refractomer to
pharmaceutical quantitative chemistry.
Discussions:
• The main principle involved in refractometry is the refraction based on the speed of the
light that passes in the different mediums.
• Light enters into the light denser medium to high denser medium at an angle, that is,
with bent. The bent in the light ray is known as the refraction.
Instrumentation:
• The instrument used for the determination of the refractive index is known as the
refractometer. There are different refractometers used for the determination of the
refractive index. They are as follows
Materials:
Dropper
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Procedure:
Data:
Conclusions:
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Name:___________________________________________ Date:_______________________
Group:___________________________________________
1. What are the different types of refractometer? Describe each and state their advantages
and disadvantages with one another.
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2. What are the uses of a refractometer?
3. List down all the parts of Abbe refractometer and describe their functions.
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Laboratory activity Assessment:
37
EXPERIMENT NO. 8
pH Determination
Objectives:
Discussions:
For electronic devices such as pH meter, it utilizes a special type of electrodes. These
electrodes used to measure hydrogen ion activity must develop a potential that varies according
to the activity of hydrogen ion in a solution (indicator electrode) and the other maintains a
constant potential called reference electrode.
Instrumentation:
pH meter
If two liquids are separated by a pH sensitive (represents the bulb part of the electrode) a
certain electrical potential will developed across the membrane. If the solution inside the bulb
contains hydrogen ion, the membrane potential may change as the hydrogen ion concentration
of the solution varies.
Materials:
Beaker 250ml
Graduated cylinder 100cc
Dropper
Stirring rod
Thermometer
2.53g of potassium bipthalate
0.88g of disodium hydrogen phosphate
0.847g monobasic potassium phosphate
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A. Procedures in preparing buffer solutions:
Buffer 4
Dissolve 2.53g of potassium bipthalate, previously dried at 110 degrees centigrade for
15mins in a carbon dioxide free water to make 250ml.
Buffer 7
Dissolve 0.88g of disodium hydrogen phosphate and 0.847g monobasic potassium
phosphate. Each dried at 110 degrees for 15mins in carbon dioxide free water.
Buffer 10
Prepare .025M sodium borate solution by dissolving 2.38g sodium boarate in 250ml
distilled water.
Prepare 0.20 M NaOH solution by dissolving .8g in 100ml distilled water.
Mix 250ml of borate solution and 27ml oh sodium hydroxide solution dilute to 500ml.
1. Turn on pH meter
2. Set the pH meter for calibration, check the temperature indicated. Wait until the machine
indicates ready.
3. First, immerse the glass electrode in buffer 4 solution. Wait until the machine indicates
ready. Record the reading.
4. Immerse the glass electrode in a beaker containing distilled water for washing purposes.
5. Repeat procedure this time using buffer 7 solution.
6. Record your data and placed each buffer solution in separate containers and label them
accordingly.
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DATA:
Pharmaceutical product
Name of Product pH meter reading Temperature pH meter reading
before heating after heating
Conclusions:
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Name:___________________________________________ Date:_______________________
Group:___________________________________________
1. What are the different types of electrode? Give their advantages and disadvantages
2. What are the basic parts of a pH meter?
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Laboratory activity Assessment:
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Activity no. 9
Objectives:
Discussions:
Many organic substances like volatile oils, sugars, and alkaloids have capabilitiy of rotating the
plane polarized light. These substances are a function of their chemical constitution and
concentration. It helps to identify the purity and identity of these substances.
Instrumentation:
Polarimeter
The sodium light with a wavelength of 589nm is linearly polarized by means of a polarizer. This
light then passes through the sample solution to be observed through an analyzer. Optically
active substance rotates the polarization plane. By measuring the rotational angle by means of
the analyzer the concentration of the solution can now be calculated.
Matreials:
Beaker 250ml
Sucrose
Distilled water
Stirring rod
volumetric flask
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Procedure in making a sugar solution
1. Pour the solution in the sample tube. Make sure that both ends of the tube is tightly
secured to avoid spillage.
2. Connect the machine to power source and switch on . wait for the lamp to emit
yellow light.
3. Look inside the viewing field, carefully rotate the scale knob until the illuminating light
have an equal intensity.
4. Check the venier scale for zero position. Adjustment can be made to zero position.
5. Open the sample chamber and put the sample tube inside. Observe that the bulb
part of the sample is positioned in an upward direction.
6. Close the chamber; adjust the viewing field by its screw. Wait for the triple view
aspect becomes clear.
7. Manipulate the scale knob by slowly rotating it. Wait until the illumination of the
viewing field becomes clear identical.
8. Read the angle of rotation by reading the dial using a magnified lens.
9. Record data.
Formula:
[a}=ty=100a/lc
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Data
Calculations:
Conclusions:
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Name:___________________________________________ Date:_______________________
Group:___________________________________________
1. Search for a picture of a polarimeter , label its parts and give the function of each parts.
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Name of Subject:______________________ Stub Code:__________________________________
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Activity no. 10
CHROMATOGRAPHY
Objectives:
Discussions:
• By analyzing a compound, a scientist can figure out what makes up that compound.
Chromatography is a great physical method for observing mixtures and solvents.
Instrumentation:
Materials
Filter paper
Capillary tube
5mg of different dyes
Plant extract
Beakers 100ml
Chloroform
ethanol
Procedure:
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3. On the TLC plate, mark a point by measuring 1cm from the lower end.
4. Using a capillary tube apply a sample from your mixed dye solution making a spot of
about 2mm in diameter.
5. Let it dry for a few seconds then place the TLC plate inside your beaker containing the
chloroform-ethanol solvent system.
6. Cover the beaker with watch glass
7. Observed the distance in which the mobile phase travels.
8. Compute the Rf value and record your data.
Data:
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Name:___________________________________________ Date:_______________________
Group:___________________________________________
1. What are the different Chromatographic technique, describe each and give its
advantages and disadvantages.
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2. What are the major parts of an HPLC apparatus? Illustrate and label each part.
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Laboratory activity Assessment:
52
REFRENCES:
Main references:
1. Totals solutions
2. Bellingham Stanley users guide
3. Flight Pharmaceutical machinery Co. limited User’s manual for CS-4 Tablet friability
4. Lab aids
5. Electronics india PH meter Instruction manual
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