CHAPTER ONE

1.0 INTRODUCTION

The student industrial work experience scheme (siwes) is an approved skill training scheme which
forms part of the minimum academic standards in various degree scheme for all Nigerian universities to
acquire skills and experience in their various course of study.

Student Industrial Work Experience Scheme was established by the Industrial training Fund (ITF) in
1973 with the aim of bridging the gap between the skills which the labour market required with that of
those acquired by the graduate students. Since its introduction by the ITF in 1973 the Scheme has gone
through series of reforms. its management, for instance, has changed hands from the ITF to the various
regulatory AGENCIES SUCH AS National Universities Commission (NUC) National board for
Technical Education (NBTE) and National Commission for college of Education (NCCE) and now
back to the ITF again. These are the major stakeholders in (SIWES).

Consequently, SIWES Programmed was introduced into the curriculum of tertiary institutions in the
country as far back as 1974 with 748 students from 11 institutions of higher learning.

However, the scheme has over the years contributed immensely to the persona l development and
motivation of students to be able to understand the important connection between the taught and learnt
content of their academic programmed and what knowledge and skill will be expected of them on
professional practice after graduation. In recognition of the short courses and weakness in the formation
of Set graduates, particularly with respect o acquisition of relevant production skills, the industrial
training fund established the students Industrial Work Experience Scheme (SIWES) in 1973 . The
Scheme was designed to expose students to the industrial environment and enable them develop
occupational experiences so that they can readily contribute their quota to national economic and
technological development after graduation. Consequently, SIWES is a planned and structured
programmed based on stated and specific career objectives, which are geared toward developing the
occupational competencies of participants.

1
 1.1 OBJECTIVE OF THE STUDENTS INDUSTRIAL WORK EXPERIENCE
PROGRAMME

The Industrial training funds policy document no. 1 of 1973, which established SIWES outline the
objectives of the scheme. The objectives are to:

1. Provide an avenue for students in institution of higher learning to acquire industrial skills and
experience during their course of study.

2. Prepare students for industrial work situation that they are likely to meet after graduation.

3. Expose students to work methods and techniques in handling equipment and machinery that may not
be available in their institutions.

.4. Make the transition from school to the world of work carrier and enhances students contacts for later
job placements.

5. Provide students with the opportunities to apply their educational knowledge in real work situations,
thereby bridging the gap between theory and practical.

1.3 BENEFITS OF INDUSTRIAL TRAINING TO STUDENTS

The industrial attachment seeks to offer students a practical translation of the theory they have been
taught. It has also got individual benefit of linking the University to the industries, hence brightening
the employment chances of the students in the University.

Through this attachment, I have generated a good inter personal relationship through my interaction
with my supervisors and colleagues. It has also improved my working skills either under pressure with
or without supervision.

2
 CHAPTER TWO

2.0 DESCRIPTION OF BIORAJ PHARMACEUTICAL LIMITED

BIORAJ pharmaceutical limited is a private and a fully own pharmaceutical company in
Nigeria whose major responsibility is to produce or manufacture drugs of high quality and
standard of Living to the society at large with motto of your health is our concern.

2.1 LOCATION AND BRIEF HISTORY OF THE COMPANY

Bioraj Pharmaceutical Limited is an indigenous pharmaceutical company owned by Pharmacist
Bioku R.J, he graduated from university of Ibadan in 1987.The Company is located in Ilorin,
Kwara state at No. 405, Kaiama road, Ilorin. Evidence is on all the documents by the
Regulatory Agencies. The company started operation in 2006 and at present, have two outlets
and a manufacturing plant. The outlets are located in Yauri Kebbi State and Kwara State while
the manufacturing outfit is located in Ilorin, Kwara State. The plant has capacity to produce
tablets (including blistered ones) and syrups.
The company has standard laboratory with necessary equipment such as UV/visible,
spectrophotometer, microscope, colony counter, water distiller, moisture content apparatus,
analytical weighing balance, leak test apparatus, melting point apparatus, pH meter, UV/Visible
spectrophotometer, microscope, Refrigerator, colorimeter, antibiotic zone reader, autoclave, etc.
The company has successfully carried out supply to state governments, teaching hospitals, and
federal ministry of health.
The company equally has Technical and Staff as required by Law and the principal of Current
Good Manufacturing Practices (cGMP) and standard operating procedure (SOP). The company
has standard Laboratory which is well equipped for physical, chemical and microbiological
analysis for both raw materials, in-process and finished products to ensure that the
manufactured products (Drugs) from the company meet both International and local standard of
efficacy, safety and wholesomeness.

VISION

To be world class pharmaceutical manufacturing company certified by world health

organization.

3
 MISSION

To produce high quality pharmaceutical dosage form under strict adherence to cGMP rule and
ensure that our

2.2 ORGANISATIONAL CHART OF BIORAJ PHARM. IND. NIG. LTD.

Managing Director

Accountant
Superintendent Pharmacist
Sales manager

Quality Assurance Production Factory Manager

Manager Pharmacist

Micro Analyst/cGMP Store

Chemical Analyst
Officer Manager

HOD HOD HOD HOD HOD

Granulation Compressi Compounding Blistering Packaging
on

4
2.3 PRODUCTS: IT’S ACTIVE AND INDICATION/USE

Bioraj pharmaceutical Limited deals on production of solid / Syrup dosages Only and they
includes:

Products: Brand Generic name Actives Ingredients Indication/ Use

name

Biobucap Ibuprofen capsule Iburopen, Non-steroidal Anti

paracetamol and inflammatory drugs
caffine (NSAIDS) used for
pains such as
Rheumatoid arthritis

Biofenac caplet Diclofenac caplet K diclofenac and Analgesic and anti-

paracetamol pyretic

Bioragly Flagly Metronidazole Amoebicide for

diarrhoea and
Amoebic infection.

Bioramol tablets Paracetamol Acetaminophen Pain and fever reliever

tablets

Biotonic capsule Blood tonic Folic acid, FAC, For Anemia

vitamin B 2

Bioracee tablets Vitamin c Ascorbic acid To prevent scurvy

Biocipro cap Ciprofloxacin Ciprofloxacin HCL Broad Spectrum

caplet antibiotic for
infections like typhoid
fever, urinary tract
infections etc.

5
 Biolin adult Cough syrup Menthol, NH4CL, For Cough Congestion
Sodium citrate

Kisivite drop Muilti- vitamin Vitamin B12, C, A, Nutrient supplement

drops nicotinamide

2.4 DEPARTMENTS/ UNITS IN THE ESTABLISHMENT AND THEIR FUNCTIONS

There are basically five departments/Units in Bioraj Pharmaceutical Limited.

There department and their functions are briefly outlined below.

2.4.1 Administration Department: The department consists of accounting section, Auditing,

Sales and marketing.

i) Account section is concerned with financial(money) stuff of the company

ii) Auditing examines the company financial records to check that they are correct

iii) Sales and Marketing deals with how the products produced gets to market.

2.4.2 Raw Materials (Store) Department: This is the department where all pharmaceutical
products and ingredients such as chemicals, starch, paracetamol etc. Are kept safe for used at a
standard condition. Some instruments in the department include; Weighing balance
Thermometer, Relative Humidity meter. The department is partitioned into various rooms such
as;

(1) The quarantine room: This is a sub-section in the raw material department
where all incoming and supplied materials are first kept. Raw materials in this
section are yet to be tested or approved for use by the chemical analyst.
(2) Raw material loading qbay: This is a sub-section in the raw materials
department where raw materials that have been tested and approved for use are
kept. Such raw material has undergone both chemical and microbial analysis and
its potency has been confirmed.
6
 (3) Cold room: In this room, approved raw materials that are temperature specific
are kept at their specified temperatures such as vitamins e.g. vitamin Ferric
ammonium citrate, Menthol crystal. The specific temperature should always be
o
kept below 25 C.
(4) Poisonous Room: this is the room where all poisonous raw materials are kept in
order to avoid misinterpretation and to implement effective sorting. Example of
chemicals in the room are caffeine, codeine etc.
(5) Reject room: This is a room where raw materials that has failed the required tests
are kept. Raw materials in this room are known as ‘reject’ as they are not suitable
for use. Most commonly find include paracetamol because of present of 4-amino
phenol which is an impurity which blackness of paracetamol.

2.4.3 Production Department

This department is mostly known as active department of the company because it is responsible
for ensuring quality is achieved in each production stage through the activities of in-process
checks. Basically, they are responsible for the production and packaging of drugs.

It is divided into two sections (Solids and Syrup) and each section caries out different duties,
they are.

i) Dispensary Section/Weighing room: : This section is the gateway for all the raw
materials used in the production department, they normally carry out weighing and
dispensing of all raw materials with the aid of Electronic weighing balances as
specified in the batch operation.

ii) Granulation Section (Solids): This section is where granules are being prepared by
Mixing, Milling, Drying, Sieving, Crushing and Blending of the dispensed raw
materials according to the procedure set by the quality control to produce the required
product. The machines used in granulation section includes Rapid Mixer granulation,
Multi- mill machine, Fluidized bed dryer, Vibro-Sifter, Comminuting mill and
Octagonal blender.

7
iii) Compression Section: Compression is the process by which granules are turned into
solids form which can be circular called “tablets” or oblong called “caplets”. This is
done with the aid of a compressing machine that consists of a die and punch.

iv) Encapsulating section: This is where empty gelatine is filled with drug powder with
the aid of capsulation machine.

v) Coasting Section: This is where some tablets that cannot be taken directly are being
coated with coating machine some of these drugs include; ferrous sulphate, and
Ibuprofen.

vi) Blistering section: This is where compressed, coated and capsulated drugs are being
blistered. I.e. putting them into polyvinyl chloride (PVC) and aluminium foil with the
aid of blistering machine.

vii) Compounding Unit (Syrup section): This is the unit where appropriate ingredients
were being combined with aid of various tools to produced syrup drugs. Some of the
equipment presents in this unit include; Syrup mixing tank, UV water sterilizer, Filter
chamber, and filter press, Colloidal milling machine, Treated water tank and
compound tank.

viii) Filling Section: In this Section syrup produced are filled in the bottle, capped and
st
sealed. The 1 assignment of quality assurance is to make sure the environment
where production is to be take place is very clean and tidy. Distill water are been used
for the production process. The bottles are checked also, if it has crack or broken and
after filling the bottle with the product, check whether there is no particle inside. The
cap must be checked whether is sealed properly or not, also check the cap after
’
sealing whether it s leaking or not. The label and leaflet must be applied properly.

ix) Packaging Section: This is where the blistered drugs are taken to, for packaging into
packets and also shrink wrapped using shrink wrapping machine.

x) Finished Product Store: Here approved finished products are kept before it will be
conveyed to the market.

8
2.4.6 Quality Control Department

This department is otherwise known as the heart of the industry because it ensures the quality of
materials used and the finished product sold out to consumers for their consumption they are
mostly concerned with sample analysis, specifications, organization, and documentation to
ensure that the finished product and raw materials are of standard. The quality control has the
power and jurisdiction to approve or reject any component, after adequate laboratory procedures.

The quality control department is divided into Five Units, they are;

i) Che mistry Laboratory: This section/unit caries out series of test on different
products, they test for raw materials, finished drugs, running of assay of different
drugs samples, dissolution test etc. They also carries out the in-process controls such
as loss on Dryness test of granules, friability test, Disintegration test, Weight
Variation, leak test on blistered drugs etc. This role is very vital for the effective
functioning of the company in the area of quality and standardization.

ii) Microbiology Laboratory: This section caries out microbial control of production
Environment, Microbial analysis of raw materials, finished products and water. They
are also in-charge of treating, transferring and deionization of production water and
distillation of water used in laboratory analysis.

iii) In-Process unit: This is a sub-section of chemical laboratories where

production/product in-progress is monitored. Various tests such as pH, L.O.D,
running weight etc are carried out intermittently to ensure uniformity.

iv) Retention sample room: This is a section in the quality control department where
samples of each batch of products produced are kept for future purposes. This is done
to monitor the stability and the half- life of the drugs and in case of any complaints
about the product by customers so as to enable tracing the product batch and run full
analysis on it.

v) Instrumentation room: A separate instrument room, so – called control room, is

preferred, otherwise serious corrosion may spoil the costly instrument, electric supply
to the instruments should be controlled by suitable voltage stabilizer, while selecting
9
 major pieces of instrument, it should be ensured that facilities for maintenance are
available.

2.5. QUALITY ASSURANCE AND CONTROL IN PHARMACEUTICAL UNIT

The term quality assurance and control are often used to refer to ways of ensuring the quality of
a service or products. For each analytical procedure, quality assurance and control is extremely
important.
Quality assurance is process-oriented and it focuses on defect prevention while quality control
is product-oriented and focuses on defect identification. However, the objectives of a quality
assurance and control programme include:

 To document the procedures and methods of sample collections, preparations and

analysis.
 To provide assurance as to reliability of analysis using replicate samples and cross
laboratory checks.

To provide assurance as to the accuracy from using recognised reference standards.
 To provide a chain of custody of samples.
 To provide assurance as to the precision and accuracy from the duplicate samples.
Both the quality assurance and control are after quality products and t hey function to see that
the products being produced are of high quality and standards by performing both chemical and
microbial tests to attest the potency of the products.

2.6. TRAINING/ORIENTATION IN BIORAJ PHARMACEUTICAL LIMITED,

Orientation is a routine done to any new intake of the company while training is done every half
year. My first day in Bioraj Pharmaceutical Industry, I was trained/ oriented by the chemical
analyst. And the GMP manager gave me the rules and regulations of the company. Thereafter,
she took me round the company and introduced me to some of the staff present on the day of my
resumption, both senior and Junior staff, even to my fellow I.T Student that have started before
me. She also took me to different suites/sections in the production department as well as quality
control department. After which I was posted to start in chemistry laboratory section of quality
control.
10
2.7.0 GOOD MANUFACTURING PRACTICES OF THE COMPANY

Good Manufacturing Practice (GMP) is that part of quality assurance which ensures that
products are consistently produced and controlled to the quality standard appropriate for their
intended use and as required by the marketing authorization. GMP aims primarily at
diminishing the risk inherent in any pharmaceutical production. Such risks include: cross
contamination and mix-up caused by for example, false labels being put on container.
This can be analyzed in three forms:

1. Dress Code/ Personnel Hygiene.

 Washing of hands and face before entering the production area.

 Clothing yourself with the overall to ensure that the dust probably in your street clothe
does not affect the product.

 The head is covered to ensure that hair does not enter thee product.

 Bathing and use of roll on, no hard smelling perfume.

 Use of Ornaments is not allowed.

 No edible thing should be taken into production area.

2. Product handling

 Products are not to be touched with bare hand.

 A product is handled at a time.

 The product must be put in keg

 Kegs are to be covered to avoid drug reactions.

 Before any keg is used, old labels must be removed and a new one placed.

 If at the course of operation the machine develops fault, protect the product by covering
before inviting the engineering team.

11
3. Operational System

 An operator is meant to wear a good foot wear to avoid electric shock.

 A machine should be test run for some minutes before starting the process

 Check the parts to ensure they are functioning properly.

 Ensure proper alignment of the machine pulley and fan belt


Ensure that your overall does not come in co ntact with any fast moving part of the machine
to avoid accident.

 Lubricate your machines daily before use to avoid wear and tear.

2.7.1 LABORATORY SAFETY RULES OF BIORAJ PHARMACEUTICAL LIMITED

i. Non laboratory staff is not allowed to touch any reagent or equipment in the laboratory.

ii. Always put on your lab coat with cap and slippers while in the laboratory.

iii. All laboratory staff must know how to use fire extinguisher.

iv. The entire storage container must be labeled with name, concentration, dates and
signature. The entire unlabelled container should be discarded.

v. No answering of phone calls in the laboratory.

vi. Food or beverages are not to be stored or consumed in the laboratory.

vii. All acids must be stored in a glass container

viii. All materials not under use should be off the reagent desk

12
 CHAPTER THREE

3.0 ACTUAL WORKDONE IN THE QUALITY CONTROL LABORATORY

CHEMICAL LABORATORY
All Pharmaceutical units need a Chemical Laboratory for Evalution of Raw material and
Finished products. A Chemical laboratory can undertake majority of the tests for Raw material
test like Solubility, Identifications reaction, Assay, Melting range, Moisture content, pH e.t.c
also Analysis of Water, Finished product both (Human and Animal) and Reagent preparation.
These products are analyzed to know if they are safe for human use or animal consumption. The
kinds of test(s) to be carried out on these products depend on the type of product to be analyzed.
The drugs can either be in tablets, capsules, syrup and suspension.
The following are the tests carried out on sample materials and Drugs:
1. Identifications test ( Qualitative analysis)
2. Assay analysis (Quantitative analysis)
3. Dissolution test Analysis
4. Physiochemical test (Physical parameters)
In the Chemical laboratory, analysis are majorly base on three major aspect, Analysis on raw
materials and Analysis on intermediate, finished products and Analysis on water

3.1 IDENTIFICATION TESTS ON RAW MATERIALS

These tests are carried out on samples to know whether the compounds used in manufacturing
the products as claimed by the manufacturers are present or not and also to know if the product
contains any harmful/impurities compound.

Analysis of Raw Materials

For Raw material to be approved for production, it has to undergo some chemical analysis both
qualitatively and quantitatively. These analyses test for its identity, potency, solubility etc.
Examples of chemical analysis on certain raw material include;

13
 1. Ibuprofen

Aim: To ensure that the product is in accordance to the specifications given

Physiochemical properties:

 A white crystalline powder


Insoluble in water, but freely soluble in organic solvent such as ether, chloroform, ethanol
 As an acid it can react with base to form the water soluble ibuprofen salt
 Melting point is 75°c

Identification test of ibuprofen.

To 5ml of its solution, add 0.5ml of 2M acetic acid and 1.2ml of a 10% w/v solution of tannic
acid.
Observations:
A yellow white, flocculent precipitate is produced which dissolves, in 6M
ammonia, Solution;
A 10% w/v of ibuprofen solution is prepared by dissolving 10mg of its powder into 100ml of
absolute ethanol.

2. Diclofenac Sodium

14
Physiochemical Properties:
 White or slightly yellowish crystalline powder that is hygroscopic.
 It has a melting point of 2800c

 It has a boiling point of 4120c

 It has a specific gravity of 1.00-1.04

 Hygroscopic in nature

·
Solubility Test on Diclofenac Sodium
Aim: To determine the solubility of diclofenac sodium.
Apparatus: Four test tubes
Procedure:

Four test tubes were labelled and filled with cold water, boiling water, alcohol, and acetone.

 Diclofenac Sodium powder was dissolved in each testtube.

Result:
 Sparring soluble in cold water,
 Freely soluble in boiling water,

 Soluble in alcohol and

 Slightly soluble in acetone.

·
Melting point test on Diclofenac Sodium (using melting point machine).
Procedure:
 The capillary tube is filled with ¼ of the given sample of Diclofenac Na+,
 And fixed into a melting point machine.
 The machine is set at the melting point range of diclofenac sodium, which is 2800c,
 If the sample is actually diclofenac Na+, at that temperature range
the sample will melt.

 The reading of when the sample starts to melt is read and taken down.

15
 3. Paracetamol (C8H9NO2)

Action: Pain reliever(Analgesic)

Physiochemical properties:
 Paracetamol is a white crystalline powder.

Solubility Test:
 Paracetamol powder was dissolved in water, methylene chloride and ethanol
Observation:
 It was sparingly soluble in water,
 Very slightly soluble in methylene chloride and

 Freely soluble in alcohol.

·
Meltiing Point:
 When a given sample of paracetamol was filled in to the capillary tube
 And inserted into the melting point DBK machine,

Obervation:
 the sample melted at the normal melting range of paracetamol, which is 1680c-1720c.

4. Lactose

16
This is an excipient ingredient which acts as a binder in drugs (tablets).

Physiochemical properties:

 A white, very fine powder, odourless and sweet.

 Soluble in 6 parts of water, very slightly soluble in alcohol, ether and in chloroform.

Identification Test:
5ml of 5%solution was heated with 5ml of 9MNH 3 in water bath maintained at 80ºC for 10mins.
A red colour is produced.
Acidity Test:
6g of the sample was dissolved in 2ml of deionized water and boiled. After cooling, 0.3ml of
phenolphthalein solution was added. The solution turns pink.

5. Sodium Bicarbonate (NaHCO3)

Action and use: Antacid, used in treatment of electrolyte deficiency.

Physiochemical properties:

 A white, crystalline powder,

 Soluble in water, practically insoluble in alcohol,

 When heated in the dry state or in solution, it gradually changes into sodium carbonate.

 Moisture Content:1.6 /0
0

Identification test:

17
To 5ml of solution S, add 0.1ml of phenolphthalein solution R ,A pale pink colour is produced.
Heat gas is evolved and the solution becomes red. It gives there action of carbonates and
bicarbonates

Solution S: Dissolve 5.0g in 90ml of carbon dioxide free water R, and dilute to100ml with
carbon dioxide free water.

Appearance of solution: Solution S is clear and colourless

Carbonates: The PH of freshly prepared solution S, is not more than 8.6

6. Propylene glycol

IUPAC name: propan-1,2-diol

Molecular Formula: C3H8O2

Physiochemical properties:
 A clear, colourless, nearly odourless,
 Viscous liquid with a faintly sweet taste and

 Hygroscopic liquid.

Solubility: Miscible With Water, Acetone and In Chloroform.

Acidity/ Alkalinity test: 10ml of the sample was mixed with 40ml of water and 0.1ml of
bromothymolblue solution was added. The solution was greenish-yellow on adding 0.05ml of
0.1M NaOH the colour changed to blue.

18
3.2 DRUG ANALYSIS (ASSAY) OF RAW MATERIAL.
The essence of drug analysis is to know the component and amount in which the active exist in
the drug.
Aim: To ascertain the percentage content of the actives in the batches

1. Ascorbic acid (C6H8O6)

Action: It is used in the treatment of vitamin C deficiency

Physiochemical properties:

 Almost odour less crystals or a white or very pale yellow crystalline powder with an
acidic taste.

 Melting point: About 190 C.

o

 0
Dissociation Constant: pKa4.2 and 11.6(25 C)

Solubility: freely soluble in water, soluble in alcohol, practically insoluble in ether and in light
petroleum.

Acidity: 5% solution has a pH of 2.2 to 2.5

Stability: Darkens slowly on exposure to air, moisture and light. Stored in a non- metallic
container

Assay;
Reagent: 1M H2SO4, starch solution, KI, CO2
Apparatus: titration set up, beaker, funnel, standard flask
Procedure:
 0.150g of ascorbic acid was weighed into a conical flask
 10ml of 1M dilute H2SO4 was added

 80ml of CO2 free water was also added

19
 1ml of corn starch (indicator) was added

 The solution was titrated against 0.05M iodine solution until a persistent violet blue
colour was obtained.

Equation and Calculation:

Titre value was recorded

(Each 1M of 0.05M Iodine is equivalent to 8.81mg of C6H8O6)

%Assay=Titre Value X Equivalent Weight X 100

Weight of Ascorbic Acid

2. Metronidazole (C6H9N3O3)

Action; antibacterial

Physiochemical properties;

 White or slightly yellowish crystalline powder,

 slightly soluble in water, acetone, alcohol and in methylene chloride.

 Melting point; 159-163 C

o

 Content 99.0% - 101.0% (dried subst)

Assay; (procedure)

20
  0.25g of Metronidazole benzoate was weighed into a conical
 It was dissolved in 100ml of anhydrous acetic acid

 A drop of crystal violet (indicator) was added

 It was titrated with 0.1M perchloric acid

NOTE; (each 1 ml of 0.1M perchloric acid is equivalent to17.12 mg of C 6H9N3O3)

%Assay = Titer Value X Equivalent Weight X 100
Weight of Metronidazole

3. Diphenylhydraminehydrochloride; (C17H21NOHCl)

Action; histamine receptor antagonist (Relieves cough)

Physiochemical properties:

 A white crystalline powder,

 Very soluble in water and freely soluble in alcohol.

 It is photosensitive.

 Melting point:167-172 C
o

Assay; (procedure)

 0.25g of the sample was weighed and dissolved in 50ml of alcohol

 1ml of 0.01M of HCl was added

 It was then titrated with 0.1MNaOH

 (Each 1ml of 0.1M NaOH is equivalent to 29.18mg of C17H21NOHCl)

%Assay=Titre Value X Equivalent Weight X100

Weight of Diphenylhydraminehydro chloride

21
3.3.0 FINISHED PRODUCTS ANALYSIS (ASSAY).
Assay of finished product is an investigative procedure in the laboratory analysis for
quantitatively measuring the presence or amount of a target entity. The measured entity is
generally called the analyst (Wikipedia).
After the identification test is carried out on the drug sample, the said drug must pass the
ASSAY test in addition to the physical parameter test before the issuance of the drug. The aim
of this analysis is to quantify the amount of the active pharmaceutical ingredient present in the
drug sample. The method of analysis used by the analyst in the analyzing these drugs are
usually reviewed from the Standard Operating Procedure (S.O.P). The S.O.P is gotten from
either U.S.P or B.P which are standard compendia for the preparation and analysis of drugs. The
acceptable limit for Active ingredient that must be present in the drug sample is between 90%
and 110%.

3.3.1 PROCEDURE FOR FINISHED PRODUCT ANALYSIS (ASSAY)

 Carry out away on the drug sample in order to obtain the average weight of the drug (for
tablet, caplets, capsules) or determine the weight per ml of the drug sample if it is in liquid form
( suspension and syrups)

 Check the S.O.P for the method of analysis of the particular active ingredient being
worked on
 Prepare the solution of the drug sample following the method of analysis stated in the
S.O.P (which should contain the molar absorptive, or morality of reagent in titrimetric.)
 Find the weight taken by using the formula

 Calculate the dilution factor using the formula

Dilution factor = a/100 × b/c × d/e.........
Where a= First volume make up
b = Second volume make up
c = No. of mistaken from first volume make up
d = No. of mistaken from second volume make up
e = Third volume make up
22
 
Shake or somicate the final solution if stated in the S.O.P.
 FOR INSTRUMENTAL METHOD;
 Proceed to the UV-Visible Spectrophotometer. Blank machine with the solvent
used to prepare the solution of the sample. Then take at least 3 absorbance of the
prepared solution of the drug sample.

 Then calculate the %Assay:

%Assay = Absorbance of sample × 100

Absorbance of standard
 FOR TITRIMETRIC METHOD:

 The method employed in volumetric analysis, in this method a solution

from graduated vessel (burette) is added to a known volume of a second solution
until chemical reaction between the two is just completed. This is shown by
colour change known as end point or in an indicator.
 Then calculate the % Assay;
%Assay = titra value × eq. wt × factor × 100
Weight taken
These are the list of finished product analyzed
i) Bioraj Ibuprofen caplet (Titrimetric method)
ii) Bioraquine Syrup (Instrumental method)
iii) Biotonic Syrup ( Titrimetric and Instrumental method)
iv) Bioraj Ciprofloxacin Hcl caplet (Dissolution method)

1. Assay of Bioraj Ibuprofen Caplet:

Active Ingredient: Isobutyl phenyl propionic acid

Apparatus: titration set-up, filtration set-up, volumetric flask, beaker, mortar and pestle.
Reagent: 0.1M NaOH, phenolphthalein, 96% ethanol, chloroform.
23
Procedure:
 Weigh 20 caplets, find it average weight and then grind them using a mortar and a
pestle.

 From the powder, take equivalent amount containing 0.4g ibuprofen; dissolve in
20ml chloroform for 15 mins.

 Filter the solution under reduced pressure, and wash the residue with two (5 ml)
chloroform.
 Evaporate the filtrate to dryness under current air (inside the hood)
 Dissolve the solid residue in 80ml absolute ethanol
 Titrate with 0.1M NaOH using phenolphthalein as indicator.
Equation and Calculation:

The chemical equation for the titration step should be:

 Note: Each 1 ml of 0.1 M NaOH is equivalent to 20.63mg of Ibuprofen.


Weight of 20 caplets = 7.820g Average Wt= 7.820/20 = 0.391g
 Weight taken = Average wt × Equivalent wt / Active wt

Weight taken = 0.391g × 0.4g/ 400mg = 3.92g

 Titra value= 19.2ml

%Assay = 19.2ml × 0.206 × 0.99 × 100

3.92g
%Assay= 99.88%
Note: According to BP, Ibuprofen tablets should contain not less than 95% and not more than
105% of the labelled amount of Ibuprofen.

24
 2. Assay of Bioraquine syrup:

Active ingredient is chloroquine phosphate.

Instruments and Apparatus : - Analytical weighing balance, UV-Visible Spectrophotometer,

volumetric flask, beaker, funnel

Reagent:- distilled water

Standard solution: - 0.125g of chloroquine phosphate powder is weigh and is prepare in water

Sample solution: - if 5ml teaspoon contains 80mg of chloroquine, then 125ml will contains
7.8ml.

Procedure;

 7.8ml of the syrup was taken

 150ml of distilled water was added.

 The solution was shook and adjusted to 250ml in the standard flask.

 5ml of the resulting solution was diluted to100ml with distilled water

 Measure the absorbance of both standard and sample solution at max wavelength 343nm.

 Calculate the %assay of bioraquine by comparison.

Calculation and Result:

Absorbance of sample

Absorban ce of standard Abso r b a n c e o f sam p l e

0.696 0.664
0.701 0.667
0.699 0.670
25
 Averag e Wt 0.699 0.668

%Assay= 0.668 × 100

0.699
%Assay = 95.57%
Note: According to BP, the syrup should contain not less than 95% and not more than 105% of
the labelled amount.

3. Assay of Biotonic syrup.

Active ingredients: Ferric Ammonium Citrate FAC, Vitamin B2 and Folic acid

 Estimation of FAC in Biotonic syrup:

Apparatus: titration set-up, volumetric flask, conical flask, funnel, beaker

Reagents: 5M HCL, Starch indicator, Na2SO4 , KI

Sample preparation: Accurately measured quantity of the sample with 5ml of Conc. HCL acid.
Transfer to 250ml standard flask with the help of water.

Procedure:

 w
Add 15ml of potassium iodide solution (10% /v).

 Keep in the dark for 5 mins and

 Titrate the liberated iodine with 0.1M sodium thiosulphate

 Using starch paste as indicator

26
 Calculate the content of FAC in the sample considering each 1ml of FAC is equivalent to
21.5mg

Calculations and Result:

If 5ml teaspoon of biotonic contain 200mg of FAC

Then, 2.5ml will contain 100mg of FAC

2.5ml is our volume measured and the Titra value is 4.50ml

To calculate %Assay = Titre value × equivalent. Weight × factor× 100

Weight taken

%Assay = 4.50ml × 21.5mg × 0.995× 100

100mg
%Assay = 96.75%
Note: According to B.P, FAC should contain not less than 95% and not more than 105% of the
labelled amount

 Estimation of vitamin B2 (Reboflavin) in Biotonic syrup:

Apparatus and Instrument: weighing device, UV-Spectrophotometer, beaker, standard flask

w
Reagents: 0.1N NaOH, 0.1N HCL acid, 2% /v KMnO4, 30% H2O2, Phosphate buffer PH 6.0
Standard solution: 150mcg/ml of riboflavin in 0.1N hydrochloric acid
Sample solution: Measure 5ml of the syrup or equivalent weight of 15mg of riboflavin, extract
with 0.1N hydrochloric acid to make 100ml.
Procedure;
 To 2ml each of sample and standard solution, add 1 drops of phenolphthalein solution

27
 And neutralize with 0.1N NaOH. Add 10ml of buffer solution followed by 2ml of acetic
acid,
 1ml of KMnO4 solution, allow to stand for 2 minute
 Neutralize pink colour with 1M H2O2, shake vigorously and dilute to 25ml with H2O.

 Measure the absorbance of both the solution at about 244nm and calculate the result by
comparison.
Calculation and Result:

Absorbance of sample Absorbance of standard

0.867 0.876
0.877 0.879
0.878 0.880
Ave.value 0.874 0.878

%Assay= 0.874 × 100

0.878
%Assay= 99.54%
NOTE: According to B.P, Vitamin B2 should contain not less than 95% and not more than
105% of the labelled amount

Estimation of Folic acid in Biotonic Syrup;

Apparatus and Instrument: weighing balance, UV-Spectrophotometer, beaker, std flask

Reagents: 0.01NaOH, 1M H2SO4, formaldehyde solution.
Standard solution: 100mcg/ml of folic acid in 0.01N NaOH
Sample solution: Measure 5ml of the syrup and extract with 25ml of 0.01N NaOH, filter and
dilute to 50ml with water.

28
Procedure:
 To 10ml of each solution, add 13ml of 1M H2SO4 and 13ml of formaldehyde.
 Close the tube with stopper and inserted a hypodermic needle

 Heat on a water bath for 1hour, cool and dilute to 25ml with water.

 Measure the absorbance of both solution at 360nm, using H 2SO4 as Blank.

Calculation and Result:

Absorbance of Absorbance of
sample standard

0.546 0.555
0.550 0.549
Ave. value 0.552
0.548

%Assay= 0.548 × 100

0.552
%Assay= 99.28%
NOTE: According to B.P, Folic Acid should contain not less than 95% and not more than
105% of the labelled amount

3.4.0 DISSOLUTION TEST

This test is carried out in the laboratory to determine the amount of the active ingredient
released from a solid oral dosage form such as tablet or capsule using a dissolution medium.
Procedure:
Place the dissolution medium in a vessel of specified apparatus and adjust the temperature of
the medium to 37oc ± 2oc using a digital thermometer. Place the dosage unit in the apparatus
and operate the apparatus at the specified rate.
After the specified time, withdraw a specimen from the solution and perform an analysis using
a suitable method.
Example
Product Name: Bioraj Ciprofloxacin Hcl caplet
29
Medium; 0.1M HCL; 900ml

Apparatus; Spindle 2:

Speed; 50 rate per minutes

Time; 30 minute

Temperature; 37◦c

Tolerance; Not less than 80% at wavelength 276nm

(Procedure;)

Test sample ; weight accurately four caplet of ciprofloxacin caplet and transfer the caplets into
a bowl containing 900ml of 0.01M HCL.

Use spindle 2 at 50rpm for a period of 30min pipette 20ml from the solution into the 100ml
standard flask.

Standard sample; weight accurately 0.0222g of ciprofloxacin Hcl powder into 100ml standard
flask, add, shake with 50ml of 0.01M HCL acid and make up to volume with 0.01M
hydrochloric acid.

Process; read the absorbance of both the sample and standard at maximum at 275nm. Calculate
the dissolution of the caplet

Calculation and Result.

Absorbance of standard = 0.60006

Dilution factor = 25
100
Absorbance of sample @276nm = 0.58342, 0.48627, 0.63766, 0.56804, 0.56087, 0.56725

30
CALCULATION
Absorbance of sample × wt of standard × vol. of medium × dilut factor × %purity × constant
Absorbance of standard vol. dissolved 1 active weight

1. 0.56725 × 22.2 × 900 × 25 × 99 × 100 = 93.49%

0.60006 100 1 10 100 500

2. 0.56087 × 22.2 × 900 × 25 × 99 × 100 = 92.44%

0.60006 100 1 10 100 500

3. 0.63766 × 22.2 × 900 × 25 × 99 × 100 = 105.09%

0.60006 100 1 10 100 500

4. 0.56804 × 22.2 × 900 × 25 × 99 × 100 = 92.62%

0.60006 100 1 10 100 500

Note: According to BP, the caplet should contain not less than 95% and not more than 105% of
the labelled amount.

3.5.0 PHYSIOCHEMICAL ANALYSIS OF DRUG.

This test is also known as determination of p hysical parameters of a sample. Under this test,
description of the physical properties of the sample (such as shape, color, texture, viscosity, and
uniformity of weight etc). The test is carried out on tablets, capsules, syrups, and suspensions.
The agency performs this test on drugs to know if such drug complies with the acceptable
standards of the British Pharmacopeia (B.P) or United States Pharmacopeia (U.S.P).The test is
also performed on drugs that are produced in order to check if the new batch still complies with
the U.S.P/B.P standards as the previous batch. If the drug fails the physical parameters analysis,

31
it means there is something wrong with the physical parameter(s) of the drug depending on
which parameter it fails.. The physical parameter analysis include:
Drug Compliance Number Analysis for (solids and liquid)

3.5.1 METHOD OF ANALYSIS FOR DRUG COMPLIANCE NUMBER (DCN)

FOR TABLETS AND CAPLETS

 20 tablets of the sample is placed in a weighing boat

 All the 20 tablets is weighed using an analytical weighing balance to obtain the
total weight of 20 tablets
 Then the individual weights of the 20 tablets are also obtained.
 The average weight of the tablet is calculated using the formula below

 The percentage deviation is calculated using the table and the formula below
% Deviation = k x Average weight
100

AVERAGE WEIGTH OF DEVIATION

TABLETS

1.80mg or less 10.0

2. greater than 80mg but less 7.5
than 250mg

3.250mg or more 5

-The uniformity of weight is then calculated using the formula below

Upper Limit (U.L) = Average weight + % Deviation
Lower Limit (L.L) = Average weight – % Deviation
The uniformity of weight is said to be satisfactory if all the individual weights of the 20
tablets/caplets fall within the upper and the lower limit. Hence the sample has passed DCN test.

FOR CAPSULES (Hard gelatin or soft gelatin)

32
  20 capsules is placed in a weighing boat

 The total weight of the 20 capsules is taken to obtain the total gross weight

 The individual weight of each of the 20 capsules is also obtained and the empty
weights of each of them

 The empty weights subtracted from the gross weights of the individual capsules
gave their net weights

 Then the empty weights of all the 20 capsules is weighted in order obtain total
empty weight

 The total empty weight of all the 20 capsules subtracted from the total gross
weight gave the total net weigh

 The total net weight is divided by the number of capsules (20 capsules) to obtain
the average weight of a capsule.

 Then the % deviation calculated using the table and the formula below

% Deviation = k × Average
weight 100
Upper Limit = Average weight + % Deviation
Lower Limit = Average weight – % Deviation
AVERAGE WEIGHT OF DEVIATION (k)
CAPSULE

Less than 300mg 10.0

300mg or more 7.5

Example: To carry out DCN analysis on Metformin Hydrochloride tablet

Procedure:
Total weight of 20 tablets = 15.2282g
Average weight of 20 tablets = 15.2282g ÷ 20 = 0.76141g
Individual weights
33
 1. 0.7654g 6. 0.7720g 11. 0.7623g 16. 0.7427g
2. 0.7442g 7. 0.7828g 12. 0.7494g 17. 0.7837g
3. 0.7671g 8. 0.7686g 13. 0.7718g 18. 0.7724g
4. 0.7486g 9. 0.7461g 14. 0.7380g 19. 0.7656g
5. 0.7606g 10. 0.7562g 15. 0.7479g 20. 0.7586g

Average weight = 15.2282g ÷ 20 = 0.76141g

Deviation (k) from the table for tablets above = 5
% Deviation = 5 × 0.76141
100
= 0.0380705
Upper Limit (U.L) = 0.76141g +
0.0380705 = 0.7994805g
Lower Limit (L.L) = 0.76141g – 0.0380705
= 0.7233395g
Since all the individual weights fall within the upper and lower limits, uniformity of weight is
satisfactory and hence the sample has passed the DCN test

FOR SUSPENSIONS, AND SYRUPS

SUSPENSION

 The suspension is first Reconstituted with equivalent liquid such as distilled water
to the mark on the container

 The fill volume is determined with a measuring cylinder

 The pH of the suspension is taken using the pH meter

 The viscosity of the suspension is determined by viscometer

 The weight per ml is also estimated.

SYRUPS

 Determine the fill volume by using a measuring cylinder

34
  Calculate the % fill volume using

%Fill volume = Fill volume / claimed fill volume× 100

 Determine the weight per 5ml

 Determine the pH value using the pH meter

3.6.0 PREPARATION OF SOME COMMON REAGENTS USED IN THE

LABORATORY

The commonly used formulas for calculation are;

1. Preparation and standardization; it involve using chemicals and dissolving them in

appropriate solvents.

Morality = amount/mass(g) × 1000(ml)

Molecular mass volume (ml)

 Preparation of Sodium hydroxide

(NaOH) Apparatus; volumetric flask, funnel, beaker,
std flask

Strength; 2M
Calculation; molar mass= 40g/mol, volume to prepared 500ml

Morality= mass/amount (g) × 1000ml

Molar mass volume(ml)

2M= mass(g) × 1000ml

40g/mol500ml mass(g) = 40g

35
Procedure: Weigh 40g of NaOH pellet, dissolve the base in little H2O, then add more dil water
to make up the solution to the mark in standard flask. Label the bottle with the content, date and
batch number.

 Preparation of Ammonium Sulphate Solution (NH4)2SO4

Apparatus: beaker, STD flask, sample bottle

Strength: 1M

Calculation: volume to prepared 250ml, Molecular mass 132.14g/mol

Morality(1M) = mass(g) × 1000ml

132.14g/mol × 250ml

Mass (g ) = 33.04g

Procedure: weigh 33.04g of the (NH4)2SO4, dissolve the salt in water, add more water to make
up to the mark of standard flask. Label the reagent bottle with the content, date and batch
number.

2. Volumetric Reagents/solution; reagents are prepared according to the usual chemical

analytical method also solution/reagents of different strengths using concentrated
reagents (i.e molar ratio)

C1V1= C2V2

Where C1= Concentration of stock V1= volume to measured from stock

C2= Concentration required (Strenght) V2= Volume to be prepared

 Preparation of sulphuric acid (H2SO4)

Apparatus; volumetric flask, beaker, reagent bottle.

Strenght; 5M

36
Calculation; volume to prepared 1000ml and Concentrated of stock 36M H2SO4

C1V1=C2V2

V1= 1000ml × 5M

36M

V1 = 139ml

Procedure; Measure 139ml 0f sulphuric acid , add distilled water to it and make up the solution
to the mark in the standard flask, label the container with the contents, date and batch number.

Precaution: never add water to acid, but a cid to water

 Preparation of dilute Acetic acid

(CH3COOH) IUPAC Name; Ethanoic acid

Apparatus; beaker, std flask, weighing bottle

Strength; 5M

Calculation; (Glacial acetic acid) concentration of stock 14.3M and volume to prepared
1000ml

C1V1=C2V2

V2= 5M × 100ml

14.3M V1 = 350ml

Procedure; Measure 350ml of glacial acetic acid, add dil- water to make it up to the mark of the
standard flask.

37
 3.7.0 WATER TREATMENT AND WATER ANALYSIS

3.7.1 Water Treatment

Bioraj Pharmaceutical Industry gets their water supply from a borehole system. Before the water
is made use of, it goes through a water treatment plant. In this treatment plant, the water passes
through three stages of purification before usage.
a. Chemical Treatment:
The borehole water is first of all C hannelled into a 1000litres over head tank
using pipes, in each pipe has a dosing value where a so lution of 100g of soda
ash (Na2CO3) is added to the water for the removal of
non-carbonate hardness in water and to increase the pH of the water. After 5
mins a solution of 2g of chlorine is added to kill the micro-organisms present.
The reaction is allowed to take place for at least 30mins before opening the water
supply.

b. Filtration Process
The treated water is pumped into the portable water tank by passing it through the
sand filter chamber for the removal of sands and impurities that may be present
in the water. It moves to charcoal column which absorbs the taste of chlorine
and also colour, from where it moves into the micro filters for further
purification. From this point the water is made ready for consumption and use
in the factory.

c. Demineralization/Deionization
Deionised water is water that has had its mineral ions removed. From portable water
tanks, production water is passed through Deionization chamber containing
Cation resin, Anion resin and mixed bed, which provide ion exchange site for
replacement of the mineral salts in water. Deionization provides high purity
water that is generally similar to distilled water with zero conductivity.

38
 Figure 3.7.1 Water Treatment Flow Chart

3.7.2 Water Analysis (Introduction)

Nowadays it is very important that continuous water samples are being taken and analyzed. For
example, drill water can often show high concentrations of chloride and iron. The basis of
evaluation for the water quality depends on what purpose is the water used for,.
Collection of Water Sample
Water sample running from a tap must be collected using a cleaned bottle, filled and shut
immediately but before collection, the tap must allowed to run for two to three minutes so as to
release the unwanted particles stored at the mouth of the tap and filled at least half of the
volume of the sample bottle which should be immediately taken to the laboratory for analysis..
In Bioraj Pharmaceutical Ltd, Two (2) types of water are of high importance for production.
These include the deionized water and the Raw Water, for both Production and General use
respectively. These waters follow a lot of processes to ascertain purity after which several test is
carried out by Q/A Analyst to determine its fitness.

39
Water physical specification:

 Description: A Clear, Colourless, Odourless and tasteless liquid.

 It has a boiling point of 100 C

0

 Weight per ml (w/ml) = 0.996 - 1.0g/ml

The following are the tests carried out on water (both treated and raw) Physical test:
Appearance: Colourless, odourless liquid.
Hardness test
Chloride ion test
pH test
Conductivity test

I. Hardness Test: (Procedure)

100 ml of water was measured into a conical flask using measuring cylinder
2 ml of ammonium – ammonia buffer solution of pH 10.4 was added to the water.
Little Erichrome T black was added and it changes to pink colour.
2+
Then it was titrated with EDTA, blue colour was observed which shows that all the ions (ca &
2+
Mg )
Then the titre value was recorded
Calculation of the total Hardness (T.H) is given
Titre value X 1000
Volume of water measured
II. Chloride Ion Test: (Procedure )
100 ml of water was measured into a conical flask
1 ml of potassium chromate was added and yellow colour was
observed Then it was titrated with silver nitrate (AgNO3)
A trace of faded brownish/orange colour was observed
It is being calculated as:
Titre value X 1000

40
 Volume of water measured

III. pH Test:
The pH test is used to determine the potential hydrogen concentration of the water sample.
There are basically two types of pH meter which are:
(i) Digital pH meter
(ii)Movable pH meter
+
pH = -log [H ]

IV. Acidity/Alkalinity: 10 ml of freshly boiled water and cooled water in a borosilicate glass
flask was added to 0.05 ml of methyl red solution. The resulting solution must not be in any
way Red. 10 ml of the same water sample was added to 0.1ml of bromothymol blue solution,
the resulting solution must not be in any way Blue.

V. Conductivity Test:
This can be carried out using conductivity meter. The calibration is done using Potassium chloride. Potassium
chloride is a buffer that is used to zero the conductivity meter or it can be tare to zero on the meter. The main
purpose we carry out this test is to know the presence of ions present in the water sample. to zero the
conductivity meter or it can be tare to zero on the meter. The main purpose we carry out this test is to know the
presence of ions present in the water sample.

Water Parameter Range

Total hardness NMT 85
Chloride test NMT 42
pH test 5.0 -7.0
Conductivity test

41
 CHAPTER FOUR

4.0 EQUIPMENTS UTILIZED DURING INDUSTRIAL TRAINING

4.1.0 CHEMISTRY LABORATORY SECTION

This is a subsection of the quality control department where chemical analysis of both raw and
finished pharmaceutical product is carried out. Some of the equipments used include:

4.1.1 UV/VISIBLE-Spectrophotometer

UV-visible spectrophotometer is one of the most frequently employed equipment in

pharmaceutical analysis. It involves measuring the amount of ultraviolet or visible radiation
absorbed by a substance in solution. The law that governs the quantitative spectrophotometric
analysis is the Beer-Lambert law which states that the quantity of light absorbed by a
substance dissolved in a non absorbing solvent is directly proportional to the concentration of
the substance and the path length of the light through the solution. This law is accurate for
dilute solutions.

Fig.4.1: UV/visible-Spectrophotometer

Mode of operation:

Power the machine by pressing the on/off button on it

Set the appropriate wavelength

Blank machine with the solvent used to prepare the solution of the sample.

42
 Introduce the sample to the device using curvtte

Then take at least 3 absorbance of the prepared solution of the drug sample.

Record the Absorbance Display data

4.1.2 Analytical Weighing Balance

Uses: This equipment used in weighing samples (in gram or mg) such as raw material or drugs
and can also be used to determine average weight of such drugs like tablet, capsule, granules etc.

Fig.4.2: Digital Analytical Weighing Balance

Mode of Operation:
 Connect the plug to the main socket (power source).
 Power the machine by pressing the on/off button on it.
 Tare to zero by pressing the tare button on the machine.
 Place a standard known weight on the weighing pan and observe the displayed value.
 Weigh your sample and record the displayed data.

4.1.5 Melting Point Apparatus

The melting point apparatus is an instrument used to determine the temperature at which solid is
turn to liquid

43
 Fig.4.3: Melting Point Apparatus

Mode of operation:

The sample is loaded into a sealed capillary (melting point capillary)

and then placed in the apparatus, the sample is then heated and as the temperature
increases

the sample is observed to determine when the phase changes from solid to liquid occurs

This temperature range that is determined can then be averaged to be the melting point of
the sample.

4.1.6 pH Meter

A ph meter measures essentially the electro-chemical potential between a known liquid inside
the glass electrode and the unknown liquid outside.

Fig.4.4: pH Meter
44
Mode of operation:

Turn on the Apparatus

Calibrate it using buffer 6.8

Placed the Electrode into the Sample for certain minutes

Record the display value

4.6.2 Electrical Distiller

This is used in distillation of water for analytical and coating purposes. Distiller
functions using boiling, evaporation and condensation techniques. The water
obtained is referred to as distilled water.

Fig. 4.5: Distiller

Mode of operation:

Power on the apparatus

The tap is turn on, by allowing the water to flow through apparatus

45
 As the water boil, the steam is cool through the flow of cold water

The distill water is collected at the outlet tube

4.3 IN-PROCESS SECTION

This section deals mainly with the checking of drugs at intervals during production to make
sure they correspond to the company product specification.

4.3.1 Moisture Analyser

Use: This equipment is used to determine the percentage moisture content/weight loss on drying
(L.O.D) of granules.

Fig. 4.6: Moisture Analyser

Mode of Operation:
Connect the plug to the main socket.
Press the on/off button on the machine to switch on.
Open the cover and spread the granules to the surface area of the
pan. Cover the lid/cover and press the start button.
Monitor the temperature, until it reaches 100⁰C

Record the displayed percentage moisture value of the sample

46
 4.3.3 Friability Testing Machine (Friabilator)
This test is a method to determine physical strength of uncoated tablets upon exposure to
mechanical shock. The instrument is shown below.

Fig.4.7: Friability Testing Machine (Friabilator)

Mode of Operation:
Connect the plug to the main socket (power source).
Weigh 20 tablets and record this as initial weight, W1
Placed 10 tablets to each side of the Wheel
Screw back the lid tightly and set the timer to 4 minutes.
Switch on the machine and watch the tablets fall as the wheels rolls.
After 4 minutes, collect back the 20 tablets and re-weigh as final weight, W2.
Determine the percentage weight loss (% friability) using the formula:
1− 2
% weight loss = × 100
1

Where W1 = Initial weight of 20 tablets.

W2 = Final weight of 20 tablets.

Specification of friability test on tablets is 0.8%.

47
4.3.4 Hardness Tester
Use: This is an instrument used to determine the breaking point of tablet under the condition of
storage, transport and handling before usage. It is measured in Kilogramme Force (KgF).

Fig.4.8: Hardness Tester

Mode of Operation:
Screw the hardness tester indicator to zero.
Place the tablet between the Anvil and Plunger.
Turn the screw clockwise till the tablet breaks.
Note the reading through the indicator as the tablet breaks and record your data.
4.3.5 Disintegration Apparatus

Use: This apparatus is used to determine the time taken for a drug (tablets/capsules) to
0
breakdown/disintegrate into smaller particles at 37 C

Fig.4.9: Disintegration Apparatus

48
Mode of Operation:
Connect the equipment to a power source.
0 0
Set the thermostat to 37 C and Fill the 1000ml beaker with water maintained at 37 C
Introduces the tablets in the tablet rack and hold with the tablet holder.
Mount the tablet rack on the mechanical device of the apparatus perpendicular to the
beaker inside the water-bath.
Press the start button and set your stopwatch till the tablets breaks down.
As the tablets breakdown, note the time on your stopwatch and record the displayed data.

49
 CHAPTER FIVE

5.0 SUMMARY, CONCLUSION AND RECOMMENDATIONS

5.1 Summary

Having gone through the necessary training involved in student industrial work
experience scheme (SIWES) with the experience gained for six months; it is highly expedient for
me to summarize my report on the platform of what I engaged in during this period. More so, I
want to recall that during my industrial attachme nt at Bioraj Pharmaceutical Ltd, I was exposed
to series of tests and assays carried out on both raw materials and finished products which as
made me to appreciate the world of science and technology.

5.2 Conclusion

My Student Industrial Work Experience Scheme (SIWES) training with BIORAJ pharmaceutical
limited has provided an avenue for me to understand practical aspects of the theoretical
knowledge already acquired in some of the courses I have offered so far as an undergraduate of
industrial Chemistry department through the necessary verification tests carried out on water and
drugs to ensure that they are up to the expected standard for human use. SIWES has made me
acquainted to the work environment. I was also exposed to various laboratory
instruments/machines, equipment, professional work methods and ways to safe guard the work
environment in industries and various organizations. The Training has given me an opportunity
to understand some of the basic principles o f chemistry which will further enhance my
knowledge of the course. This training also gave me the opportunity to interact, share knowledge
and ideas with other students from different institutions.

5.3 Recommendation:

TO SIWES

1. The SIWES should endeavor to pay the students industrial visits regularly to ensure that the
students are being trained as expected and not used for purposes other than why they are there.
They should also ensure that the environment is conducive for learning and pay the students
allowances as when due to motivate the students.

50
2. The training should be well coordinated so that undergraduates can be exposed to the actual
work experience taking place in their respective fields.

3. The Institution should also help in securing placement for students.

TO BIORAJ

1. Regular maintenance of instruments and apparatus should be carried out in order to keep
them in good condition
2. A more efficient method should be devised for the disposal of waste chemicals used and
workshops should be organized from time to time in order to sensitize workers of the importance
of taking safety precautions when working in the laboratory.

3. BIORAJ should endeavor to organize seminars for their SIWES student intakes in order to
get them familiar with the processes of the laboratories before they start working in the
laboratories because each student has different level of exposure

5.4 PROBLEMS ENCOUNTERED DURING THE PROGRAMME.

Distance: It takes a lot of resources and time to get to my place of attachment from my
place of abode. This contributed to poor state of health as I straggle to wake up early to
meet up with 7am being their startment time.

Having less time for myself as the company Operates from Monday to Friday without
observing public holidays.

No compensation from the company

REFERENCES

Federal Military Government (1990). Industrial Training Fund, Jos, Nigeria.

ITF (1973). Policy Document No 1. Industrial Training Fund, Jos, Nigeria

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British pharmacopoeia volume I and II 2017Grysell Ramos, 1998.

Chemical raw material analysis book, 2nd Edition.

Olakunle Okelola, 2012 Good manufacturing practices for pharmaceutical manufacturers green
rd
guide 3 edition.

Onyechi, J. and Onyeka, J., 2011. Hand book of pharmaceutical facility auditor and validation
practice

Bioraj pharmaceutical manual test procedure (in process log book)

Shah, D.H., 2010. Standard operation guidelines U.S pharmacopeia 2005 edition

Allen, C. R. quoted in Craig, R. L. (1987). Training a Development Handbook

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