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Table of Contents

Page experiment Name Score Date


no. no.

1 Weight variation tests

2 Friability test

3 Hardness and thickness


test for tablets

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:____________________________

1
Activity no. 1

Weight Variation

Objectives:

To be able to demonstrate knowledge and application of statistic in quality control

To be able to demonstrate statistical calculation derived from the data taken.

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.

2. Place all the data in the table provided.

3. Calculate the following

a. average weight
b. % weigh variation
c. standard deviation
d. relative standard deviation
e.relative average deviation

2
B. Procedure

1. Using a graphing paper, prepare a control chart by plotting your data.


a. assign x-axis as the number of each sample
b. assign y-axis as the weight of each sample

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.

3
Laboratory activity Assessment:

Name of Subject:___________________________Stub Code:__________________________________

Name:____________________________________________ Group no.________________________


Date:_______________________

Title of lab Activity:___________________________________________________________________


Activity no:__________________

Section:_________________________________ Group no:__________________________________

Criteria Did not Unsatisfactory= Proficient= Advance=


perform=0
a. Results Absent Figures, graphs, tables All figures,graphs All figures, graphs,
Did not perform contains errors or are and tables are and tables are
poorly correctly complete and well
constructed.missing presented but presented
titles, captions or there are areas
numbers, units are missing or needs
missing. improvement.
b. Discussion Absent Very incomplete, Almost all results All results have
Did not perform incomplete have been been discussed
interpretation of correctly with comparison
results, unable to interpreted and to the principles
compare data with discussed but still that governs the
principles needs activity. Good
improvement understanding of
the activity
c. Conclusions Absent Conclusion is missing; All conclusions All important
Did not perform there is a missing of have been drawn conclusions have
some important but could be been discussed
points stated better thoroughly,
Students shows
understanding
d. Grammar Absent There are more than There are less All grammar,
Did not perform 10 grammar, spelling than 3 grammar, spelling and
and sentence spelling and sentence
construction error sentence construction are
construction. correct, no error,
Mature readable advance style of
style writing.
e. Appearance Absent Sections out of order All sections are in All sections are
and formatting Did not perform Hand written not order but still clear,well
legible needs an formatted and
Sloppy formatting improvement very readable.

4
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

Tablet Friability Test

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.

It is therefore important that the tablet is formulated to withstand such stress.

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.

5
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.

Friability is usually measured by the use of Roche friabilator or tumbler tester.

INSTRUMENTATION:

Friabilator

 Makes use of a tumbling apparatus where tablets are exposed to rolling and repeated
shocks from free fall within the apparatus.

 conditions: 100 revolutions in 4 minutes

SPECIFICATIONS:

 A. if the weight is > 650mg per tablet use 10 samples.

 B. If the weight is<650mg per tablet use 20 samples.

There should not be any damaged or broken tablet.Not More Than 1% loss in weight.

Calculations:

 % weight Loss= initial weight - Final weight x100

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

6
Data GENERIC TABLET Branded TABLET
Name: Name:
initial weight
final weight
% weight loss

CALCULATIONS:

CONCLUSIONS:

Name:___________________________________________ Date:_______________________

Group:___________________________________________

7
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.

8
Laboratory activity Assessment:

Name of Subject:___________________________Stub Code:__________________________________

Name:____________________________________________ Group no.________________________


Date:_______________________

Title of lab Activity:___________________________________________________________________


Activity no:__________________

Section:_________________________________ Group no:__________________________________

Criteria Did not Unsatisfactory= Proficient= Advance=


perform=0
a. Results Absent Figures, graphs, tables All figures,graphs All figures, graphs,
Did not perform contains errors or are and tables are and tables are
poorly correctly complete and well
constructed.missing presented but presented
titles, captions or there are areas
numbers, units are missing or needs
missing. improvement.
b. Discussion Absent Very incomplete, Almost all results All results have
Did not perform incomplete have been been discussed
interpretation of correctly with comparison
results, unable to interpreted and to the principles
compare data with discussed but still that governs the
principles needs activity. Good
improvement understanding of
the activity
c. Conclusions Absent Conclusion is missing; All conclusions All important
Did not perform there is a missing of have been drawn conclusions have
some important but could be been discussed
points stated better thoroughly,
Students shows
understanding
d. Grammar Absent There are more than There are less All grammar,
Did not perform 10 grammar, spelling than 3 grammar, spelling and
and sentence spelling and sentence
construction error sentence construction are
construction. correct, no error,
Mature readable advance style of
style writing.
e. Appearance Absent Sections out of order All sections are in All sections are
and formatting Did not perform Hand written not order but still clear,well
legible needs an formatted and
Sloppy formatting improvement very readable.

9
Activity no. 3

Hardness and Thickness tests for Tablets

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:

1. Tablet Hardness tester

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.

a. Erweka hardenss tester


b. Scleuniger hardness tester
c. Strong Cobb Hardness tester
d. Stokes Monsanto Hardness tester

Acceptable ranges for Stokes Monsanto Hardness tester

a. 4 to 10 kg for ordinary compressed tablets


b. 2 kg for sublingual tablets
c. 2kg for chewable tablets
d. 10 kg for buccal tablets

10
Tablet thickness

Venier Caliper or Thickness Gauge

Materials:

8 chewable tablets

8 ordinary tablets

8 sublingual tablets

YPJ-200B type Pill hardometer

Venier caliper

Procedure for Tablet Hardness test:

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.

Procedure for Table thickness test:

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.

11
HARDNESS TEST

Name Hardness Newton Hardness Newton Hardness Newton Average Average


of 1 in Kg 2 in Kg 3 in Kg hardness Newton
sample

THICKNESS TEST

Name of sample Thickness 1 in Thickness 2 in Thickness 3 in Average


mm. mm mm

COMPUTATIONS:

12
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.

13
2. Interpret the following Venier Caliper readings:

a. b.

c. d.

e. f.

14
Laboratory activity Assessment:

Name of Subject:____________________________ Stub Code:__________________________________

Name:____________________________________________ Group no.________________________


Date:_______________________

Title of lab Activity:___________________________________________________________________


Activity no:__________________

Section:_________________________________ Group no:__________________________________

Criteria Did not Unsatisfactory= Proficient= Advance=


perform=0
a. Results Absent Figures, graphs, tables All figures,graphs All figures, graphs,
Did not perform contains errors or are and tables are and tables are
poorly correctly complete and well
constructed.missing presented but presented
titles, captions or there are areas
numbers, units are missing or needs
missing. improvement.
b. Discussion Absent Very incomplete, Almost all results All results have
Did not perform incomplete have been been discussed
interpretation of correctly with comparison
results, unable to interpreted and to the principles
compare data with discussed but still that governs the
principles needs activity. Good
improvement understanding of
the activity
c. Conclusions Absent Conclusion is missing; All conclusions All important
Did not perform there is a missing of have been drawn conclusions have
some important but could be been discussed
points stated better thoroughly,
Students shows
understanding
d. Grammar Absent There are more than There are less All grammar,
Did not perform 10 grammar, spelling than 3 grammar, spelling and
and sentence spelling and sentence
construction error sentence construction are
construction. correct, no error,
Mature readable advance style of
style writing.
e. Appearance Absent Sections out of order All sections are in All sections are
and formatting Did not perform Hand written not order but still clear,well
legible needs an formatted and
Sloppy formatting improvement very readable.

15
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:

Disintegration test for tablets and capsules

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 stated by USP

 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:

1. Basket rack assembly

a. 6 open ended transparent tubes


b. 10 mesh wire cloth at the bottom
c. disks
2. 1000ml low form beaker

3. Thermostatic control for heating fluid

4. Device for raising and lowering the basket

16
Apparatus A

Use apparatus A for tablets and capsules that are not greater than 18 mm.

The apparatus A consists of

• a basket-rack assembly

• a 1000 mL low-form beaker

• 138–160 mm in height and having an inside diameter of 97–115 mm for the immersion
fluid

• a thermostatic arrangement for heating the fluid between 35 °C and 39 °C

• 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.

Method for test A apparatus

 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

For larger tablets and capsules use apparatus B.

The apparatus B consist of:

• 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.

17
• The tubes are held vertically by 2 separate and superimposed rigid plastic plates 97 mm
in diameter and 9 mm thick with 3 holes

Method for test B

 Test 6 tablets or capsules either by using 2 basket-rack assemblies in parallel or by


repeating the procedure.

 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

1. Temperature must be maintained at 37 degrees centigrade

2. a. Distilled water

b. Simulated Gastric fluid TS

c. Simulated Intestinal fluid TS

Materials:

Disintegration apparatus with beaker

6 generic tablet or capsules

6 branded tablet or capsules

Specifications:

All tablets should disintegrate completely

Procedures:

 Refer to the procedures presented depending on what type of apparatus will be used.

18
DATA:

Generic TABLET/ TABLET/ TABLET/ TABLET/ TABLET/ TABLET/


CAPSULE CAPSULE CAPSULE CAPSULE CAPSULE CAPSULE
NO. 1 NO. 2 NO. 3 NO. 4 NO. 5 NO. 6
Disintegration
time

DATA:

Branded TABLET/ TABLET/ TABLET/ TABLET/ TABLET/ TABLET/


CAPSULE CAPSULE CAPSULE CAPSULE CAPSULE CAPSULE
NO. 1 NO. 2 NO. 3 NO. 4 NO. 5 NO. 6
Disintegration
time

Remarks/conclusion:

19
Name:___________________________________________ Date:_______________________

Group:___________________________________________

1. Compare the difference between USP method and BP method for disintegration test for
enteric coated tablets.

20
2. Search for the diagram of Apparatus A and B for disintegration test. Paste them in the
space provided and label accordingly.

21
Laboratory activity Assessment:

Name of Subject:____________________________ Stub Code:__________________________________

Name:____________________________________________ Group no.________________________


Date:_______________________

Title of lab Activity:___________________________________________________________________


Activity no:__________________

Section:_________________________________ Group no:__________________________________

Criteria Did not Unsatisfactory= Proficient= Advance=


perform=0
a. Results Absent Figures, graphs, tables All figures,graphs All figures, graphs,
Did not perform contains errors or are and tables are and tables are
poorly correctly complete and well
constructed.missing presented but presented
titles, captions or there are areas
numbers, units are missing or needs
missing. improvement.
b. Discussion Absent Very incomplete, Almost all results All results have
Did not perform incomplete have been been discussed
interpretation of correctly with comparison
results, unable to interpreted and to the principles
compare data with discussed but still that governs the
principles needs activity. Good
improvement understanding of
the activity
c. Conclusions Absent Conclusion is missing; All conclusions All important
Did not perform there is a missing of have been drawn conclusions have
some important but could be been discussed
points stated better thoroughly,
Students shows
understanding
d. Grammar Absent There are more than There are less All grammar,
Did not perform 10 grammar, spelling than 3 grammar, spelling and
and sentence spelling and sentence
construction error sentence construction are
construction. correct, no error,
Mature readable advance style of
style writing.
e. Appearance Absent Sections out of order All sections are in All sections are
and formatting Did not perform Hand written not order but still clear,well
legible needs an formatted and
Sloppy formatting improvement very readable.

22
Activity no. 5

SPECTROMETRY: UV-Vis SPECTROPHOTOMETER

Objectives:

 To be able to learn the principles of spectrophotometry and its application to


pharmaceutical quantitative analysis.
 To learn the basic parts of a spectrometer, its function and operation.

Discussion:

• UV-Vis or Ultraviolet-visible spectroscopy refers to absorption spectroscopy or


reflectance spectroscopy in the ultraviolet-visible spectral region.

• Measurement of the attenuation of a beam of light after it passes through a sample or


after reflection from a sample surface.

• Absorption spectroscopy refers to spectroscopic techniques that measure


the absorption of radiation, as a function of frequency or wavelength, due to its
interaction with a sample.

• Absorption spectrometry encompasses the wavelength regions; ultraviolet (200–380


nm), visible (380–780 nm), near infrared (780 nm to 2.5 m) and infrared (2.5–40 m).

• Electromagnetic radiation is commonly treated as a wave phenomenon, characterized


by a wavelength or frequency.

• 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).

• Wavelength is the distance between adjacent peaks , and may be designated in


meters, centimeters or nanometers (10-9 meters).

Instrumentation:

Spectrometer UV-VIS

Procedure:

23
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:

Name of sample Absorbance reading USP specifications

Conclusions:

24
Name:___________________________________________ Date:_______________________

Group:___________________________________________

1. Illustrate the basic parts of a Spectrometer, label and explain each part and its function.

25
2. What are the uses of UV-Vis Spectrometer?

3. What is the different types/model of spectrometer?

26
Laboratory activity Assessment:

Name of Subject:___________________________Stub Code:__________________________________

Name:____________________________________________ Group no.________________________


Date:_______________________

Title of lab Activity:___________________________________________________________________


Activity no:__________________

Section:_________________________________ Group no:__________________________________

Criteria Did not Unsatisfactory= Proficient= Advance=


perform=0
a. Results Absent Figures, graphs, tables All figures,graphs All figures, graphs,
Did not perform contains errors or are and tables are and tables are
poorly correctly complete and well
constructed.missing presented but presented
titles, captions or there are areas
numbers, units are missing or needs
missing. improvement.
b. Discussion Absent Very incomplete, Almost all results All results have
Did not perform incomplete have been been discussed
interpretation of correctly with comparison
results, unable to interpreted and to the principles
compare data with discussed but still that governs the
principles needs activity. Good
improvement understanding of
the activity
c. Conclusions Absent Conclusion is missing; All conclusions All important
Did not perform there is a missing of have been drawn conclusions have
some important but could be been discussed
points stated better thoroughly,
Students shows
understanding
d. Grammar Absent There are more than There are less All grammar,
Did not perform 10 grammar, spelling than 3 grammar, spelling and
and sentence spelling and sentence
construction error sentence construction are
construction. correct, no error,
Mature readable advance style of
style writing.
e. Appearance Absent Sections out of order All sections are in All sections are
and formatting Did not perform Hand written not order but still clear,well
legible needs an formatted and
Sloppy formatting improvement very readable.

27
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:

•Optimization of therapeutic effectiveness during product development and stability assessment.

•Routine assessment of production quality to ensure uniformity between production lots.

•Assessment of ‘bioequivalence’, that is to say, production of the same biological availability


from discrete batches of products from one or different manufacturers.

•Prediction of in-vivo availability, i.e. bioavailability (where applicable).

Instrumentation;

Dissolution apparatus single basket type


UV-Vis spectrometer

Materials

Thermometer
Pipette
Volumetric flask
Rubber aspirator
Mefenamic generic 500mg
Mefenamic Branded 500mg

28
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)

Group no. Conc. After 5 min interval temperature

Reference (Branded)

Group no. Conc. After 5 min interval temperature

Spectral reading

Group no. Absorbance of Absorbance of % of drug after 5


sample reference min interval

29
Computation:

Conclusions:

30
Name:___________________________________________ Date:_______________________

Group:___________________________________________

1. What are the different types of Dissolution apparatus? Give each of their description. List
their advantages and disadvantages.

31
Laboratory activity Assessment:

Name of Subject:___________________________ Stub Code:__________________________________

Name:____________________________________________ Group no.________________________


Date:_______________________

Title of lab Activity:___________________________________________________________________


Activity no:__________________

Section:_________________________________ Group no:__________________________________

Criteria Did not Unsatisfactory= Proficient= Advance=


perform=0
a. Results Absent Figures, graphs, tables All figures,graphs All figures, graphs,
Did not perform contains errors or are and tables are and tables are
poorly correctly complete and well
constructed.missing presented but presented
titles, captions or there are areas
numbers, units are missing or needs
missing. improvement.
b. Discussion Absent Very incomplete, Almost all results All results have
Did not perform incomplete have been been discussed
interpretation of correctly with comparison
results, unable to interpreted and to the principles
compare data with discussed but still that governs the
principles needs activity. Good
improvement understanding of
the activity
c. Conclusions Absent Conclusion is missing; All conclusions All important
Did not perform there is a missing of have been drawn conclusions have
some important but could be been discussed
points stated better thoroughly,
Students shows
understanding
d. Grammar Absent There are more than There are less All grammar,
Did not perform 10 grammar, spelling than 3 grammar, spelling and
and sentence spelling and sentence
construction error sentence construction are
construction. correct, no error,
Mature readable advance style of
style writing.
e. Appearance Absent Sections out of order All sections are in All sections are
and formatting Did not perform Hand written not order but still clear,well
legible needs an formatted and
Sloppy formatting improvement very readable.

32
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:

• Refractometry is the method of measuring the refractive index of substances. Refractive


index is defined as the ratio of the speed of light in a vacuum to the speed of light in
another substance is defined as the index of refraction or refractive index (n) for the
substance.

• 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

• Traditional handheld refractometer: The main principle involved in this refractometer is


the measurement of the critical angle. It is comprised of the lenses and prisms to project
the black line on the glass when the sample is placed between the measuring prism and
the plate

• Abbes refractometer: This is a benchtop refractometer, designed by Ernst Abbe, which


provides high accuracy. In this refractometer, the sample is held between the
illuminating prism and the refracting prism. A light source is allowed through the
illuminating prism and the detector is placed behind the refracting prism.

Materials:

5 different volatile oils

Dropper

33
Procedure:

1. Turn the locking knob and raise the upper prism.


2. Place a few drops of the sample on the lower prism and close the upper prism.
3. Secure the locking knob and be sure that the sample evenly covers the prism and is free
of bubbles.
4. Open the shutter on the upper prism and raise the mirror shutter on the lower prism. This
will allow light pass to the upper prism to the sample.
5. For opaque sample, use the reflection mode.
6. Close the shutter on the upper prism and lower the mirror shutter on the lower prism.
This will allow light to reflect to the underside part of your sample.
7. Look in the eyepiece and rotate to focus the scale and the borderline
8. Adjust the dispersion knob to remove color until it will create a sharp border line.
9. Rotate the control knob to align th borderline with the center crosswise.
10. Record the reading.

Data:

Sample Refractive index Refractive index USP

Conclusions:

34
Name:___________________________________________ Date:_______________________

Group:___________________________________________

1. What are the different types of refractometer? Describe each and state their advantages
and disadvantages with one another.

35
2. What are the uses of a refractometer?

3. List down all the parts of Abbe refractometer and describe their functions.

36
Laboratory activity Assessment:

Name of Subject:____________________________________________________ Stub


Code:__________________________________

Name:____________________________________________ Group no.________________________


Date:_______________________

Title of lab Activity:___________________________________________________________________


Activity no:__________________

Section:_________________________________ Group no:__________________________________

Criteria Did not Unsatisfactory= Proficient= Advance=


perform=0
a. Results Absent Figures, graphs, tables All figures,graphs All figures, graphs,
Did not perform contains errors or are and tables are and tables are
poorly correctly complete and well
constructed.missing presented but presented
titles, captions or there are areas
numbers, units are missing or needs
missing. improvement.
b. Discussion Absent Very incomplete, Almost all results All results have
Did not perform incomplete have been been discussed
interpretation of correctly with comparison
results, unable to interpreted and to the principles
compare data with discussed but still that governs the
principles needs activity. Good
improvement understanding of
the activity
c. Conclusions Absent Conclusion is missing; All conclusions All important
Did not perform there is a missing of have been drawn conclusions have
some important but could be been discussed
points stated better thoroughly,
Students shows
understanding
d. Grammar Absent There are more than There are less All grammar,
Did not perform 10 grammar, spelling than 3 grammar, spelling and
and sentence spelling and sentence
construction error sentence construction are
construction. correct, no error,
Mature readable advance style of
style writing.
e. Appearance Absent Sections out of order All sections are in All sections are
and formatting Did not perform Hand written not order but still clear,well
legible needs an formatted and
Sloppy formatting improvement very readable.

37
EXPERIMENT NO. 8

pH Determination

Objectives:

 To be able to learn and apply the principles of pH determination.


 To be able to learn the basic parts, functions of pH meterand its application to
pharmaceutical quantitative chemistry.

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

38
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.

Procedure for pH meter calibration using prepared buffer solutions.

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.

Test for Pharmaceutical preparations.

1. Use any generic pharmaceutical solutions.


2. Place 50ml of the liquid in a 100ml beaker
3. Test the ph of this solution using pH meter. Record the pH reading
4. Subject the solution to heat using water bath, but do not boil it.
5. While still warm, determine its pH. Observe and record your reading.

39
DATA:

Buffer solution data:


Solutions pH meter reading Temperature
Buffer 4
Buffer 7
Buffer 10

Pharmaceutical product
Name of Product pH meter reading Temperature pH meter reading
before heating after heating

Conclusions:

40
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?

41
Laboratory activity Assessment:

Name of Subject:________________________ Stub Code:__________________________________

Name:____________________________________________ Group no.________________________


Date:_______________________

Title of lab Activity:___________________________________________________________________


Activity no:__________________

Section:_________________________________ Group no:__________________________________

Criteria Did not Unsatisfactory= Proficient= Advance=


perform=0
a. Results Absent Figures, graphs, tables All figures,graphs All figures, graphs,
Did not perform contains errors or are and tables are and tables are
poorly correctly complete and well
constructed.missing presented but presented
titles, captions or there are areas
numbers, units are missing or needs
missing. improvement.
b. Discussion Absent Very incomplete, Almost all results All results have
Did not perform incomplete have been been discussed
interpretation of correctly with comparison
results, unable to interpreted and to the principles
compare data with discussed but still that governs the
principles needs activity. Good
improvement understanding of
the activity
c. Conclusions Absent Conclusion is missing; All conclusions All important
Did not perform there is a missing of have been drawn conclusions have
some important but could be been discussed
points stated better thoroughly,
Students shows
understanding
d. Grammar Absent There are more than There are less All grammar,
Did not perform 10 grammar, spelling than 3 grammar, spelling and
and sentence spelling and sentence
construction error sentence construction are
construction. correct, no error,
Mature readable advance style of
style writing.
e. Appearance Absent Sections out of order All sections are in All sections are
and formatting Did not perform Hand written not order but still clear,well
legible needs an formatted and
Sloppy formatting improvement very readable.

42
Activity no. 9

Rotatory power: Polarimetry

Objectives:

 To be able to learn and apply the principles of polarometry.


 To be able to learn the basic parts, functions of a polarimeterand its application to
pharmaceutical quantitative chemistry.

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

43
Procedure in making a sugar solution

1. Weight 50 grams of sugar


2. Add distilled water to make 100ml
3. In a 100ml volumetric flask, transfer 50ml of the sugar solution. Add distilled water to the
mark.
4. Let it stand for 5mins. Then determine its optical rotation using polaimeter.

Procedure for Polarimeter

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

C=concentration of the analyte or solute express as g/100c


L=length of the tube express in dm
a= is the degree recorded
[a]= rotation of the sample
T=temperature

44
Data

Concentration of the solution:


Length of tube:
Reading no. 1=
Reading no.2=
Reading no.3=
Average reading=

Calculations:

Conclusions:

45
Name:___________________________________________ Date:_______________________

Group:___________________________________________

1. Search for a picture of a polarimeter , label its parts and give the function of each parts.

2. What are the uses of a polarimeter?

3. Explain the complete principle behind polarimetry.

Laboratory activity Assessment:

46
Name of Subject:______________________ Stub Code:__________________________________

Name:____________________________________________ Group no.________________________


Date:_______________________

Title of lab Activity:___________________________________________________________________


Activity no:__________________

Section:_________________________________ Group no:__________________________________

Criteria Did not Unsatisfactory= Proficient= Advance=


perform=0
a. Results Absent Figures, graphs, tables All figures,graphs All figures, graphs,
Did not perform contains errors or are and tables are and tables are
poorly correctly complete and well
constructed.missing presented but presented
titles, captions or there are areas
numbers, units are missing or needs
missing. improvement.
b. Discussion Absent Very incomplete, Almost all results All results have
Did not perform incomplete have been been discussed
interpretation of correctly with comparison
results, unable to interpreted and to the principles
compare data with discussed but still that governs the
principles needs activity. Good
improvement understanding of
the activity
c. Conclusions Absent Conclusion is missing; All conclusions All important
Did not perform there is a missing of have been drawn conclusions have
some important but could be been discussed
points stated better thoroughly,
Students shows
understanding
d. Grammar Absent There are more than There are less All grammar,
Did not perform 10 grammar, spelling than 3 grammar, spelling and
and sentence spelling and sentence
construction error sentence construction are
construction. correct, no error,
Mature readable advance style of
style writing.
e. Appearance Absent Sections out of order All sections are in All sections are
and formatting Did not perform Hand written not order but still clear,well
legible needs an formatted and
Sloppy formatting improvement very readable.

47
Activity no. 10

CHROMATOGRAPHY

Objectives:

 To be able to learn and apply the principles of chromatography technique.


 To be able to learn the application of chromatography to pharmaceutical quantitative
chemistry.

Discussions:

• Some materials appear homogenous, but are actually a combination of substances.

• For example, green plants contain a mixture of different pigments

• In many instances, we can separate these materials by dissolving them in an


appropriate liquid and allowing them to move through an absorbent matrix, like paper.

• Chromatography is a method used by scientists for separating organic and inorganic


compounds so that they can be analyzed and studied.

• 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.

• Is a physical method of separation in which the component tobe separated are


distributed between two phases, one of which is stationary (stationary phase) while the
other (the mobile phase) moves in a different direction.

Instrumentation:

Thin layer chromatography Plates

Materials

Filter paper
Capillary tube
5mg of different dyes
Plant extract
Beakers 100ml
Chloroform
ethanol
Procedure:

1. Mix 5ml chloroform and 2ml ethanol in a beaker


2. Cover the inside part of the beaker with filter paper

48
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:

Testing for different Dyes


Sample distance travelled distance travelled Rf value
by solute by solvent
Dye 1
Dye 2
Dye 3

Testing for different sugar solutions


Sample distance travelled distance travelled Rf value
by solute by solvent
Sucrose solution
Lactose solution
Glucose solution

Testing for different plant extract solutions


Sample distance travelled distance travelled Rf value
by solute by solvent
Plant extract

49
Name:___________________________________________ Date:_______________________

Group:___________________________________________

1. What are the different Chromatographic technique, describe each and give its
advantages and disadvantages.

50
2. What are the major parts of an HPLC apparatus? Illustrate and label each part.

51
Laboratory activity Assessment:

Name of Subject:___________________________Stub Code:__________________________________

Name:____________________________________________ Group no.________________________


Date:_______________________

Title of lab Activity:___________________________________________________________________


Activity no:__________________

Section:_________________________________ Group no:__________________________________

Criteria Did not Unsatisfactory= Proficient= Advance=


perform=0
a. Results Absent Figures, graphs, tables All figures,graphs All figures, graphs,
Did not perform contains errors or are and tables are and tables are
poorly correctly complete and well
constructed.missing presented but presented
titles, captions or there are areas
numbers, units are missing or needs
missing. improvement.
b. Discussion Absent Very incomplete, Almost all results All results have
Did not perform incomplete have been been discussed
interpretation of correctly with comparison
results, unable to interpreted and to the principles
compare data with discussed but still that governs the
principles needs activity. Good
improvement understanding of
the activity
c. Conclusions Absent Conclusion is missing; All conclusions All important
Did not perform there is a missing of have been drawn conclusions have
some important but could be been discussed
points stated better thoroughly,
Students shows
understanding
d. Grammar Absent There are more than There are less All grammar,
Did not perform 10 grammar, spelling than 3 grammar, spelling and
and sentence spelling and sentence
construction error sentence construction are
construction. correct, no error,
Mature readable advance style of
style writing.
e. Appearance Absent Sections out of order All sections are in All sections are
and formatting Did not perform Hand written not order but still clear,well
legible needs an formatted and
Sloppy formatting improvement very readable.

52
REFRENCES:

Main references:

1. Watson, David G.Pharmaceuticals analysis: a textbook for pharmacy students and


pharmaceutical chemists, 4th ed. Singapore: Elsevier. 2017.
2. Knevel, A.M. and Digangi, F.E., Jenkin’s Quantitative Pharmaceutical Chemistry.USA:
Mc Graw Hill. 1977.
3. Lerma,Norma. Drug and Cosmetic Quality control with Instrumentation, 2 nd edition.
Manila, Phil: UST Publishing House,1996
4. Gennaro, Alfonso R. Remington: The Science and Practice of Pharmacy. 19 th edition. 2
volumes.Pennsylvania, USA: Mack Publisihing Co.1995
5. Hamilton,Leicester F. and Stephen G. Simpson.Quantitative Chemical Analysis 12 th
edition.New York: The Macmillan Company.1971
6. United States Pharmacopeial Convention,Inc. (USPCI) The Unites States Pharmacopiea
(USP) XXIII and the National Formulary (NF) XV111. Twinbrook Parkway.
Rockville.1995

Instruments manual refrences:

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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