TECHNICAL REPORT ON SIX MONTHS STUDENT INDUSTRIAL

WORK EXPERIENCE SCHEME (SIWES)

AT

TUYIL PHARMACEUTICALS LIMITED

NO 22, NEW YIDI ROAD, IREWOLEDE, ILORIN, KWARA STATE.

Prepared by

OLADEPO, BAKIAT SALEWA

MATRIC NO: NOU211171745

PROGRAMME: B.Sc. Chemistry

FACULTY: SCIENCE

YEAR OF STUDY: 2024 [300LEVEL]

COURSE TITLE: INDUSTRIAL TRAINING (SIWES)

COURSE CODE: CHM394

MOBILE TELEPHONE: 07055664903

EMAIL: nou211171745@noun.edu.ng

FROM: 18TH MARCH 2024 TO 30TH AUGUST 2024

IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE

AWARD OF BACHELOR OF SCIENCE (B.SC. HON) IN CHEMISTRY.

NATIONAL OPEN UNIVERSITY OF NIGERIA UNIVERSITY VILLAGE

PLOT 91 CADASTRAL ZONE, NNAMDI AZIKIWE EXPRESS WAY JABI-
ABUJA.
ILORIN STUDY CENTRE

1
 ACKNOWLEDGMENT

My greatest appreciation and honor goes to God almighty whom without, I would not even have the cause
to write this report, my parents Mr. and Mrs. Oladepo thank you very much for your support,
encouragement, prayers and financial assistance. May God continue to bless you.

To my SIWES based supervisors/instructors Mr. Samson Onuoha, Mr. Aremu J.O, Mrs. Elizabeth, The
Managing Director of TUYIL, Mr. Arowolo for giving me the opportunity to undertake my industrial
training at the firm and all Tuyil Pharmaceutical Industry's Staff and security personnel. I thank you all.

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 ABSTRACT

Student industrial work experience scheme (SIWES) is a compulsory skills acquisition training program
designed to give university undergraduate in Nigeria appropriate practical knowledge in practical work
place environment in their respective disciplines during their course of study and to under the industrial
application of the theoretical knowledge that they have acquired. It also serves as a means to develop
occupational competences that would facilitate their fitting into the world of work after graduation. I was
fortunate to serve my six (6) month SIWES Program at TUYIL Pharmaceutical Industry Limited, a well
recognized Pharmaceutical firm that offers indigenous drug manufacturing services in Nigeria. This
report is a comprehensive summary of all that I learnt and achieved throughout my SIWES program at
TUYIL Pharmaceutical Industry Limited. The section one gives a brief introduction to the history and
organizational structure of TUYIL Pharmaceutical Industry Limited, section two contains skills,
practices, operation and maintenance training received, section three discusses adequate coverage and
experiment carried out, section four highlights the activities carried out at the water treatment plant
while section section five which is the last section contains the achievement of SIWES, conclusion,
acknowledgement, reference and recommendations.

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 TABLE OF CONTENT

TITLE PAGE

ACKNOWLEDGMENT

ABSTRACT

TABLE OF CONTENT

SECTION ONE

INTRODUCTION

AIM, OBJECTIVE AND HISTORICAL BACKGROUND OF SIWES PROGRAM

BRIEF HISTORY OF TUYIL PHARMACEUTICAL INDUSTRY LIMITED ILORIN

COMPANY'S ORGANIZATIONAL CHART

SECTION TWO

SKILLS ACQUIRED IN VARIOUS DEPARTMENT OF THE ORGANIZATION

QUALITY CONTROL DEPARTMENT

DETAILS OF WORKS DONE IN THE QUALITY CONTROL DEPARTMENT

DETERMINATION OF ABSORPTION OF SYRUP DRUGS USING SPECTROPHOTOMETER

PREPARATION OF BUFFER

TYPES OF BUFFER SOLUTIONS

THE PHYSICAL METHODS OF PREPARING A BUFFER

INDICATORS USED IN QUALITY CONTROL PHARMACEUTICAL LAB

PREPARATION OF INDICATORS

SECTION THREE

TABLE OF EXPERIMENTS DONE, TEST AND RESULTS

STANDARDIZATION OF SOLUTIONS

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STANDARDIZATION OF NAOH WITH KHP

STANDARDIZATION OF HCL WITH NAOH

ASSAY

ASSAY OF ASCORBIC ACID IN VITAMIN C SYRUP

ASSAY OF ASPIRIN TABLET

SECTION FOUR

DETAILS OF WORK DONE IN THE WATER TREATMENT PLANT

INTRODUCTION TO WATER TREATMENT PLANT

BIOLOGICAL TREATMENT METHODS

DETERMINATION OF HARDNESS OF WATER

THE DETERMINATION OF HARDNESS PROCESS

DETERMINATION OF CALCIUM

PREVENTION OF INTERFERENCE

SECTION FIVE

CONCLUSION

RECOMMENDATIONS

ACHIEVEMENT AND OUTCOME OF SIWES

REFERENCE

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 SECTION ONE

1.0 INTRODUCTION

1.1 INTRODUCTION TO SIWES

The student industrial work experience scheme (SIWES) is the accepted skill training program, which
form part of the approved minimum academic standards in the various degree programs for all the
Nigerian universities. It is an effort to bridge the gap existing between theory and practice of engineering
and technology, science, agriculture, medical, management and other professional education program in
the Nigeria tertiary institutions. It is aimed at exposing student to machine and equipment, professional
work methods and ways of safe guarding the work areas and workers in industries and other
organizations.

The scheme is a tripartite program, involving the students, the universities and the industry
(employers of labor). It is funded by the federal government of Nigeria and jointly coordinated by the
Industrial Training Fund (ITF) and the National Universities Commission (NUC).

1.2 AIMS AND OBJECTIVES OF SIWES

1. Prepare students for the work situation they are likely to meet after graduation.

2. Provide an avenue for students in the Nigerian universities to acquire industrials skills and
experience in their course of study.

3. To make the transition from the university to the world of work easier and thus enhance students
contacts for later job placement.

4. Enlist and strengthen employers' involvement in the entire educational process of preparing
universities graduate for employment in industries.

5. Expose students to work methods and techniques in handling equipment and machines that may
not be available in the universities.

1.2.1 HISTORY OF SIWES

Student industrial work experience scheme (SIWES) was setup in 1973 by the federal
government direction with the urge that each student in higher institution of learning should undergo in
order to satisfy their university requirement.

In 1971, the (ITF) was established with zonal office (branched) all over the country, the program
(SIWES) afford student of tertiary institution the opportunity of being familiar and at the same time being
exposed to the experience that is needed and how to handle equipment and machinery that are not reached
by student in school. It makes the student appreciate the theory being thought in class by applying the
practical aspect of it in their various places of attachment.

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1.3 BRIEF HISTORY OF TUYIL PHARMACEUTICAL INDUSTRY LIMITED ILLORIN,
KWARA STATE.

TUYIL Pharmaceutical industry limited is one of the well-recognized indigenous drug manufacturing
companies in Nigeria. Tuyil of written philosophy is that it is a trusted name in pharmaceuticals industry
and have always try in it day to day activities and has tried to maintain its trusted philosophy.

Tuyil is one of the prestigious pharmaceutical companies in Nigeria which is fully approved by
the NAFDAC. It was registered in May 1996 and founded by Mr. Oluwole Awotuyi with 36 workers and
4 management team. It was formally located at No; 22 stadium road Ilorin where the whole activities
were carried out until it moves to it permanent site at No: 22 new Yidi road Ilorin. The administrative
section is headed by Mr. Arowolo.

Tuyil was commissioned by his Excellency Dr. Bukola Saraki and late Dora Akunyili former DG
of NAFDAC. The first product to be produced in this company was paracetamol; it was later preceded
into producing human and veterinary drugs. Raw materials used by the company are being imported from
Germany through its agent in Lagos while other raw materials were procured locally from Lagos and
some local parts of the country. The company product has a wide range of market network in various part
of the country where they are sold by the sales representatives.

1.4 THE COMPANY ORGANISATIONAL CHART

Tuyil pharmaceutical company is headed by a chairman/CEO followed by supertendant pharmacist who

is followed by a quality assurance manager followed by a personnel manager, production pharmacist, and
also we have quality control manager under which there are chemical analyst and a microbiologist.

The chemical analysts are usually graduates from chemistry, chemical engineering or
microbiology. And under the production pharmacist we have the production supervisor and under the
personnel manager we have the secretary, clerk, security men. It also consists of several departments such
as the production department, maintenance department, administrative department, quality control
department, and warehousing department.

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1.4.1 TUYIL ORGANOGRAM OF DRUG PLANT FACTORY

Fig 1.1

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 SECTION TWO

SKILLS ACQUIRED IN VARIOUS DEPARTMENT OF THE ORGANIZATION

2.0 QUALITY CONTROL DEPARTMENT

It consists of chemical laboratory and microbiology laboratory. It is the heart beat of the company
because it controls all the department in the organization, the department oversees sampling testing and
analyzing of raw materials to intermediate and finished product so that the product meets the required lay
down standards.

2.1 DETAILS OF WORKS DONE IN THE QUALITY CONTROL DEPARTMENT

2.1.1 Calibration and the use of pH meter

A pH meter is an electric device used to measure hydrogen-ion activity (acidity or alkalinity) in solution.
A pH meter must be calibrated for it to be able to measure the pH of a particular solution accurately. A
pH meter can be calibrated following the steps below,

Procedure: The pH Mode was selected and the temperature control knob was set to 25°C, the calibration
knob was also adjusted to 100%. The electrode was rinsed with deionized water and it was blot dry using
a piece of tissue. The electrode was placed in the solution of pH 7 buffer and the display was allowed to
stabilize, then the display was set to read 7 by adjusting calibration 1 and then the electrode was removed
from the buffer.

The electrode was rinsed with deionized water and blot dried using a piece of tissue. The electrode was
placed in the solution of pH 2 buffer, the display was allowed to stabilize and, then, the display was later
set to read 2 by adjusting calibration 2 and now the electrode was removed from the buffer. The electrode
will now be rinsed with deionized water and blot dried using a piece of tissue, now the pH meter has been
calibrated. The calibrated pH meter can now be used to measure the pH of a particular solution by making
sure that the meter is set to the pH Mode and the temperature was adjusted to 25°C. The electrode is
placed in the sample to be tested and the pH of the solution appears in the display, the display is allowed
to stabilize before any readings can be taken.

Below is a diagram of a pH meter

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Fig 2.1

2.2 DETERMINATION OF ABSORPTION OF SYRUP DRUGS USING

SPECTROPHOTOMETER

A spectrophotometer is an instrument that measures the amount of photons (the intensity of light)
absorbed after it passes through sample solution. With the spectrophotometer, the amount of a known
chemical substance (concentrations) can also be determined by measuring the intensity of light detected.

Spectrophotometers are designed to transmit light of narrow wavelength ranges. A given

compound will not absorb all wavelengths equally-that's why things are different colors (some
compounds absorb only wavelengths outside of the visible light spectrum, and that's why there are
colorless solutions like water). Because different compounds absorb light at different wavelengths, a
spectrophotometer can be used to distinguish compounds by analyzing the pattern of wavelengths
absorbed by a given sample. Additionally, the amount of light absorbed is directly proportional to the
concentration of absorbing compounds in that sample, so a spectrophotometer can also be used to
determine concentrations of compounds in solution. Finally, because particles in suspension will scatter
light (thus preventing it from reaching the light detector), spectrophotometers may also be used to
estimate the number of cells in suspension.

When studying a compound in solution by spectrophotometry, The sample is poured in a sample

holder called a cuvette and I is placed in the spectrophotometer. Light of a particular wavelength passes
through the solution inside the cuvette and the amount of light transmitted (passed through the solution
Transmittance) or absorbed (Absorbance) by the solution is measured by a light meter. While a
spectrophotometer can display measurements as either transmittance or absorbance.

The spectrophotometer work with the principles of Beer and Lambert

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1. The Beer's law which states that the absorbance is directly proportional to the concentration (c) of the
solution of the sample used in the experiment.

Aαc 1.1

2. The Lambert's law states that absorbance is directly proportional to the length of the light path (II),
which is equal to the width of the cuvette.

Aα1 1.2

Combining Equations 1.1 and 1.2:

Aαc1

The picture of how a spectrophotometer works is shown below

Fig 2.2

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2.3 PREPARATION OF BUFFER

A buffer solution is an aqueous solution consisting of a mixture of a weak acid and its conjugate base, or
vice versa. Its pH changes very little when a small amount of strong acid or base is added to it.

Buffer solutions

A solution whose pH is not altered to any great extent by the addition of small quantities of either strong
acid (H+ ions) or a strong base (OH- ions) is called the buffer solution. It can also be defined as a solution
of reserve acidity or alkalinity which resists change of pH upon the addition of small amount of acid or
alkali.

A buffer solution is one which resists changes in pH when small quantities of an acid or an alkali are
added to it.

Acidic buffer solutions

An acidic buffer solution is simply one which has a pH less than 7. Acidic buffer solutions are commonly
made from a weak acid and one of its salts - often a sodium salt.

A common example would be a mixture of ethanoic acid and sodium ethanoate in solution. In this case, if
the solution contained equal molar concentrations of both the acid and the salt, it would have a pH of 4.7
it wouldn't matter what the concentrations were, as long as they were the same.

You can change the pH of the buffer solution by changing the ratio of acid to salt, or by choosing a
different acid and one of its salts.

Alkaline buffer solutions

An alkaline buffer solution has a pH greater than 7. Alkaline buffer solutions are commonly made from a
weak base and one of its salts.

A frequently used example is a mixture of ammonia solution and ammonium chloride solution. If these
were mixed in equal molar proportions, the solution would have a pH of 9.25. Again, it doesn't matter
what concentrations you choose as long as they are the same.

Types of buffer solutions:

There are two types of buffer solutions,

(1) Solutions of single substances: The solution of the salt of a weak acid and a weak base.

Example: ammonium acetate, (CH, COONH, NH, CN) act as a buffer.

(ii) Solutions of Mixtures: These are further of two types,

(a) Acidic buffer: It is the solution of a mixture of a weak acid and a salt of this weak acid with a strong
base.

Example: CH, COOH + CH, COONa

(b) Basic buffer: It is the solution of a mixture of a weak base and a salt of this weak base with a strong
acid.

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Example: NH4OH + NH4CI

(2) Buffer action: Buffer action is the mechanism by which added H + ions or OH- ions are almost
neutralized; so that pH practically remains constant. Reserved base of buffer neutralizes the added H + ions
while the reserved acid of buffer neutralizes the added OH- ions.

(3) Buffer capacity is a measure of the efficiency of a buffer in resisting changes pH. Conventionally,
the buffer capacity ( ) is expressed as the amount of strong acid or base, in gram-equivalents, that must
be added to 1 liter of the solution to change its pH by one unit.

Examples of buffer solutions

(i) Phthalic acid + potassium hydrogen phthalate

(ii) Citric acid + sodium citrate.

(iii) Boric acid + borax (sodium tetraborate).

(iv) Carbonic acid (H₂CO₃) + sodium hydrogen carbonate (NaHCO3). This system is found in blood and
helps in maintaining PH of the blood close to 7.4 (PH value of human blood lies between 7.36-7.42; a
change in pH by 0.2 units may cause death).

(v) NaH2PO4 + Na2PO4

(vi) NaH2PO4 + NaHPO4

(vii) Glycerine + HCI

(viii) The PH value of gastric juice is maintained between 1.6 and 1.7 due to buffer system.

All buffers rely on having two components: a substance that will neutralize with excess acidity and a
substance that will neutralize excess alkalinity (basicity). Thus a weak acid and its conjugate base are
typically the two substances used in buffers. Background The basic equation governing buffers is called
the Henderson-Hassel Baich equation, after the two scientists that independently published it. This
equation is derived from the expression for the equilibrium constant of a weak acid. For instance, if the
weak acid is acetic acid, the ionization of acetic acid can be written into hydrogen ions and acetate ions:

HC₂H₂O2(aq) H+(aq) +C2H3O2 – (aq)

Which becomes the equilibrium constant (Ka) expression:!

Ka=[H+][C₂H₃O₂"] [HC₂H₃O₂]

The Ka can be looked up any reference; the text gives the Ka of acetic acid to be 1.8 x 10-5.

The Henderson-Hasselbalch equation is given in the text (in a slightly different form; you can use that one
or the one given below to derive the various concentrations needed for your recipe. I'll define the "pKa" in
a manner analogous to pH: pKa= - log10 Ka

Thus, the pKa of acetic acid is = - log10 (1.8×10-5) = 4.74.

So to make a buffer of a certain pH, the general Henderson-Hasselbalch equation can be used to.

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The general equation of Henderson-Hasselbalch is given below

pH=pKa+log10 [base] [acid]

2.5 THE PHYSICAL METHODS OF PREPARING A BUFFER

If there is only one of the buffer components available, the buffer preparation is done by titration method.

a) In case of availability of weak acid or weak base only. An acidic buffer is made by titrating the weak
acid by strong base, and a basic buffer is made by titrating the weak base by strong acid until the desired
pH is obtained.

b) In case of availability of the salt of weak acid or base only. An acidic buffer is made by titrating the
salt of weak acid by strong acid, and a basic buffer is made by titrating the salt of weak base by strong
base until the desired pH is obtained.

PREPARATION OF ACETATE BUFFER pH 4.6

5.4g of sodium acetate was weighed and dissolved in 50ml of water, 2.4g of glacial acetic acid and it was
dilute to 100ml with water.

PREPARATION OF AMMONIUM BUFFER pH 10.9

5.4g of ammonium chloride was weighed and dissolved in 20ml of water, 35ml of ammonium and it was
diluted to 100ml with water.

PREPARATION OF AMMONIUM BUFFER pH 10.9

6.75g of ammonium chloride was weighed and dissolved in ammonia and it was made up to 100 with
water.

PREPARATION OF ACETATE BUFFER pH 3.4

5 volumes of 0.1 sodium acetate was mixed with 95 volume of 0.1M acetic acid.

PREPARATION OF ACETATE BUFFER pH 3.5

25g of ammonium acetate was weighed and dissolved in 25ml of water and 38ml of 7M HCL, the pH was
adjusted to 3.5 with either 2M HCL or 6M ammonia and it was diluted with 100ml of water.

3.0 INDICATORS USED IN QUALITY CONTROL PHARMACEUTICAL LAB

INDICATORS: These are solutions used to provide a visual determination of the end point of a reaction
these maybe a change in colour of the formation of precipitate.

TYPES OF INDICATORS USED IN QUALITY CONTROL PHARMACEUTICAL LAB

1. Acid-Base indicator

2. Redox

3. Complexometric

4. Precipitation

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1. ACID-BASE INDICATOR: they are weak acid or weak bases. They include; Bromocresol green,
cresol red, crystal violet, methyl Orange, methyl red, phenolphthalein, thymol blue etc. An example this
type of titration is the assay for aspirin.

2. REDOX-INDICATOR: Under a definite colour change at a specific electrode potential include;

Nitrophenatrolene, diphenylamine, indigo-carmine, methylene blue, feroin example of this type is the
assay of paracetamol.

3. COMPLEXOMETRIC INDICATORS: these are ironochromic dyes that undergo a definite colour
change in the presence of specific metal ion. They are water soluble which include erichrome black T,
xylenon orange, murexide, erichrome blue, methylthymol blue, naphtol green. Example of this type is the
assay in the determination of calcium and magnesium salt. It can also be used to determine zinc.

4. PRECIPITATION: Precipitate from solution in a readily visible form at or near the equivalent point
of titration, it includes fluorescence, eosin starch solution.

2.6 PREPARATION OF INDICATORS

1. ACID-BASE INDICATORS:

Methyl orange

Methyl orange is one of the indicators commonly used in titrations. It is an orange crystalline powder
slightly soluble in water and practically insoluble in ethanol. In an alkaline solution, methyl orange is
yellow and the structure is shown below:

The yellow form of methyl orange

The solution can be prepared by dissolving 0.1g of methyl orange powder in 80ml of water and it is
diluted to 100ml with ethanol.

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Phenolphthalein

Phenolphthalein is slightly soluble in water and usually is dissolved in alcohols for use in experiments. It
is a weak acid, which can lose H ions in solution. The phenolphthalein molecule is colorless, and the
phenolphthalein ion is pink.

The phenolphthalein solution can be prepared by dissolving 1.1g of phenolphthalein powder with
sufficient amount of ethanol and making to 100ml with sufficient amount of ethanol.

Methyl red

Methyl Red is a maroon red crystal azo dye. Methyl Red is a pH indicator and changes color at a pH of
5.5.

Methyl red is an orange yellow crystalline powder which is soluble in ethanol and insoluble in water

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The solution can be prepared by dissolving 0.1g of methyl red in 50ml of ethanol and sufficient amount of
water is added to make up to 100ml.

2. REDOX INDICATORS:

Methylene Blue

Methylene Blue is a dark green or bronze grey crystalline powder which is freely soluble in water and
soluble in ethanol.

The methylene blue solution is prepared by dissolving 0.1g of methylene blue powder by 100ml of water.

INDIGO CARMINE

Indigo carmine, or 5, 5'-indigodisulfonic acid sodium salt, is an organic salt derived from indigo by
sulfonation, which renders the compound soluble in water. It is a blue or violet blue powder or blue
granules with a coppery luster sparingly soluble in H₂O and practically insoluble in ethanol.

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The solution can be prepared by mixing 1ml of concentrated HCL and 99ml of 20% v/v nitrogen free
sulphuric acid, 0.2g of indigo carmine was added.

3. PRECIPITATION INDICATOR:

STARCH IODINE PAPER

The strips filter paper was dipped in 100ml of iodide free starch solution containing 0.1g of potassium
iodate. The solution is now drained and allowed to cool.

Hence, the starch iodide paper is ready for use.

EOSIN POWDER: It is a red powder soluble in H₂O and ethanol

Preparation: Dissolve 0.1g of eosin powder in 100ml of H₂O

4. COMPLEXOMETRIC INDICATORS:

MURESIDE

It is a brownish red crystalline powder sparingly soluble in cold water and soluble in hot water and
practically insoluble in ethanol. It is also soluble in the solutions of KOH or NaOH giving blue color.

The murexide solution can be produced by dissolving 0.1g of murexide powder in 100ml of KOH or
NaOH.

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 SECTION THREE

TABLE OF EXPERIMENTS DONE, TEST AND RESULTS

3.1 STANDARDIZATION OF SOLUTIONS

Standardization: is the process of determining the exact concentration (molarity) of a solution.

Titration is one type of analytical procedure often used in standardization. In a titration, an exact volume
of one substance is reacted with a known amount of another substance.

The point at which the reaction is complete in a titration is referred to as the endpoint. A chemical
substance known as an indicator is used to indicate (signal) the endpoint. The indicator used in this
experiment is phenolphthalein. Phenolphthalein, an organic compound, is colorless in acidic solution and
pink in basic solution.

Materials: Burette, Pipette, retort stand, stirrers, volumetric flask and beaker

3.2 Standardization of NaOH with KHP

1. The burette is cleaned by rinsing with several portions (about 10 mL) of tap water. (The burette is clean
enough when water droplets do not cling to the inner surface.) This rinse water can be poured down the
drain.

2. About 150 mL of the NaOH solution is obtained in a clean, dry 400 mL beaker. Covered with a watch
glass.

3. The burette is cleansed with three portions (about 5 mL) of the NaOH solution. Each NaOH was
drained, rinsed and discarded into the waste container located under the hood.

4. The burette was filled with NaOH to slightly above the zero mark and the burette was clamped up
vertically.

5. The air bubbles was removed from the tip of the burette by draining the NaOH into a small beaker. The
NaOH level was read to within ± 0.02 mL and The value was recorded and the initial base reading on the
data sheet. (It is not necessary to have the NaOH level at exactly the 0.00 mL. mark. Anywhere below
0.00 mL. will suffice. What is important, is to record this initial NaOH reading to two decimal places.)

6. A clean 250 ml. beaker was weighed to +0.01 g. 0.6 to 0.7 g of KHP was added (potassium acid
phthalate; HKCH404) and the beaker was reweighed with the contents to ± 0.01 g. The mass was
recorded on the data sheet.

7. All the KHP was dissolved in water by adding about 30 mL of distilled water to the beaker and stirred
with a glass rod. (If necessary, the solution can be warmed to dissolve all the solid acid.) The solution is
now transferred into a clean 250 mL Erlenmeyer flask and the beaker was rinsed twice with about 5 mL,
of distilled water to make sure all of the acid has been transferred to the flask.

8. 3 to 4 drops of phenolphthalein indicator were added to the KHP solution in the Erlenmeyer flask.

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9. The flask containing the acid solution and indicator was placed under the burette And NaOH from the
burette was added to the flask with swirling until the color of the solution in the flask is a faint pink. This
faint pink color should last only 45 to 60 seconds. There should be a one-drop difference between when
the solution is colorless and when it is pink. If too much base is added (that is, if there is "over-shooting"
the endpoint), the solution should be discarded and the titration is repeated. A white piece of paper placed
under the flask will aid in the color detection.

10. When the proper end point is reached, final NaOH volume is read and recorded to within ±0.02 mL.

11. The contents of the Erlenmeyer flask was discarded into the waste container located under the hood.

12. The titration procedure was repeated the second time by following steps 4-11.

3.3 Standardization of HCl with NaOH

1. The NaOH burette was refilled. The NaOH level was read to within ±0.02 mL, the value was recorded
and the initial base reading on the data sheet.

2. A clean, but not necessarily dry, 250 mL. Erlenmeyer flask was obtained, and using the burette labeled
"HCI" (located at the back of the room), Approximately 25.00 mL of the HCl acid solution was
transferred into the flask. The initial and final acid burette readings was read and recorded to ± 0.02 mL.
It is not necessary to deliver exactly 25.00 mL of HCI into the flask. What is important is that the volume
of HCl delivered into the flask is known to two decimal places.

3. 3 to 4 drops of phenolphthalein indicator were added to the HCl solution in the Erlenmeyer flask.

4. The flask containing the acid solution and indicator was placed under the burette and NaOH was added
from the burette to the flask with swirling until a phenolphthalein endpoint is reached. There should be a
one-drop difference between when the solution is colorless and when it is pink. If too much base is added
(that is, if there's "over-shooting" the endpoint), the solution was discarded and repeat the titration.

5. When the proper end point is reached, the final NaOH volume was read and recorded to within ±0.02
mL.

6. The contents of the Erlenmeyer flask was discarded and recorded into the waste container located
under the hood. The titration procedure was repeated and recorded a second time by following steps 1-
5.

3.4 ASSAY

Assay: An assay is an analysis done to determine:

The presence of a substance and the amount of that substance present. Thus, an assay may be
done for example to determine the level of thyroid hormones in the blood of a person suspected of being
hypothyroid (or hyperthyroid).

The chemical or pharmacological potency of a drug. For example, an assay may be done of a
vaccine to determine its potency.

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3.4.1 ASSAY OF ASCORBIC ACID IN VITAMIN C SYRUP

Ascorbic Acid is a naturally occurring compound with antioxidant property. It can either be a white solid
(pure sample) or appear yellowish (impure sample). It dissolves well in water to give mildly acidic
solution. There are two types of ascorbic acid. They are;

i. L-ascorbic acid

ii. D-Ascorbic acid.

Ascorbic Acid is the active ingredient in the production of vitamin C syrup. From the name 'a' means No
and "scorbutic" means Scurvy. Scurvy is the disease caused by the deficiency of vitamin C.

AIM:

To show whether the claim complies with the specification or standard.

REAGENT:

Starch mucilage, 1M H2SO4, CO2 free water, 0.05M iodine solution, Sample.

PRINCIPLE:

The principle of this experiment is redox reaction

APPARATUS:

Burette, Pipette, Dropper, Spatula, Weighing Balance, Beaker and conical flask.

PREPARATION OF STARCH MUCILAGE

 1g of soluble starch is weighed and then dissolves with 5ml of water.

 95ml of boil water (CO₂ free water) was added to make it up to 100ml plus continuous stirring.

PROCEDURE FOR THE ASSAY OF VITAMIN C

 0.05M of iodine solution was poured into the burette to mark.

 5ml of the sample was taking and poured into a conical flask.

 25ml of 1M H₂SO₄ was added to it.

 100ml of CO2 free water was also added.

 Finally, 1ml of starch mucilage was added as indicator followed by thorough shaking.

 Titrate until a blue-violet color was obtained.

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RESULT:

Burette Reading (cm3) 1st Titration

Initial Burette Reading(cm3) 0.0

Final burette Reading(cm3) 11.4

Table 3.1

CALCULATION:

Given; Each ml of 0.05M iodine solution is equivalent to 0.008806g ascorbic acid according to British
Pharmacopoeia;

 1ml of 0.05M iodine = 0.008806g

 Convert 0.008806g to mg

 0.008806g8.806mg

 When 1ml of 0.05M iodine solution = 8.806mg of ascorbic acid

 11.4ml of 0.05M iodine solution = (11.4×8.806) mg of ascorbic acid

 =100.3884mg of ascorbic acid

 =100.4mg of ascorbic acid

 Hence, 5ml of the sample (Vitamin C) contain 100.4mg of ascorbic acid.

CHEMICAL SIGNIFICANCE

 As antioxidant.

 To prevent and to treat scurvy in patients.

 It is used as coenzyme in the synthesis of collagen and nor epinephrine.

CONCLUSION

 High quantity of vitamin C is obtained from fruits and vegetables. Therefore, vitamin C from
fruits and vegetables is preferable to vitamin C from cooked foods or drugs.

 Take adequate vitamin C and experience its good health benefits.

3.4.2 ASSAY OF ASPIRIN TABLET

Analysis of Aspirin Tablets

Aspirin is an analgesic and antipyretic drug. The main constituent of aspirin tablets is an organic acid.

Objectives:

22
The object of this experiment is to determine the percentage of 2-ethanoylhydroxybenzoicacid
(acetylsalicylic acid) in aspirin tablets. A known amount of standard sodium hydroxide solution is used in
excess to hydrolyze a known mass of aspirin tablets.

CH3COOC6H4COOH + 2NaOH CH3COONa + HOC6H4COONa + H20

The unused sodium hydroxide which remains is then titrated with standard acid. The amount of alkali
required for the hydrolysis can then be calculated, using the above equation. The amount in moles of the
acid which has been hydrolyzed can be found. This method can be described as performing a "Back
Titration."

Materials and Apparatus

1. One Pipette filler

2. One 25 cm Pipette

3. One 50 cm3 burette

4. One funnel

5. Two 25 cm3 conical flask

6. One stand and clamp (burette)

7. Two 150 cm3 beakers

8. One 250 cm3 standard flask

9. Bunsen Burner Kit10. Digital Scale11.Stop Watch12.Lab coat, goggles, gloves

Procedure

a. 1.5g of Aspirin tablets was weighed into a 250 cm3 conical flask. 25 cm3 of 1.0 M sodium
hydroxide by pipette was added to initiate the hydrolysis of the aspirin tablet, diluting with
approximately the same volume of distilled water. The flask was warmed over a tripod and gauze
for ten minutes to complete the hydrolysis.

b. Cool the reaction mixture was cooled and transferred with washings to a 250 cm3 volumetric
flask, it was dilute to the mark with distilled water making sure that the contents of the flask are
well mixed by repeated shakings.

c. Titrate 25 cm3 portions of the diluted reaction mixture with the standard 0.050 M sulphuric acid
provided, using phenol red indicator until two or three consistent results Are obtained.

Brand: X

Given: [H2SO4] = 0.050 mol dm-3 [NaOH] 1.027 mol dm-3

Calculation:

Mass of aspirin 1.092 g (3 tablets)

23
Average vol. of H2SO4 used (in procedure c) 14.56 cm3

No. of moles of H₂SO₄ used 0.050 × 1000

56.147.28×10-4H2SO4+ 2NaOH Na2SO4+ 2H2O

No. of moles of excess NaOH

(25 cm3, in conical flask)-2 ×7.28 ×10-4-1.456×10-3

No. of moles of excess NaOH in the volumetric flask (250cm3)=1.456×10-3×10-1.456×10-2

No. of moles of NaOH in the original solution (procedure)=1.027 ×100025-0.02568

No. of mole of NaOH reacted with aspirin =0.02568-0.01456=0.01112

CH3COOC6H4COOH(s) + 2NaOH (aq) CH3COONa (aq) + HOCH4COONa (aq) + H2O (1)

No. of moles of acetyl salicylic acid-201112.0-0.00556

Mass of acetyl salicylic acid -0.00556×180-1.0008 (g) Mass of acetyl salicylic acid in each tablet
30008.1-0.3336 (g)

% by mass of acetyl salicyclic acid in the tablet-092.10008.1×100%-91.65%

24
 SECTION FOUR

DETAILS OF WORK DONE IN THE WATER TREATMENT PLANT

4.0 INTRODUCTION TO WATER TREATMENT PLANT

I was introduced to the water treatment plant. Water is the most widely used substance, raw
material or starting material in the production, processing and formulation of pharmaceutical products. It
has unique chemical properties due to its polarity and hydrogen bonds. This means it is able to dissolve,
absorb, adsorb or suspend many different compounds. These include contaminants that may represent
hazards in themselves or that may be able to react with intended product substances, resulting in hazards
to health.

Control of the quality of water throughout the production, storage and distribution processes,
including microbiological and chemical quality, is a major concern.

Unlike other product and process ingredients, water is usually drawn from a system on demand,
and is not subject to testing and batch or lot release before use.

Assurance of quality to meet the on-demand expectation is, therefore, essential. Additionally,
certain microbiological tests may require periods of incubation and, therefore, the results are likely to lag
behind the water use.

Control of the microbiological quality of WPU is a high priority. Some types of microorganism
may proliferate in water treatment components and in the storage and distribution systems. It is crucial to
minimize microbial contamination by proper design of the system, periodic sanitization and by taking
appropriate measures to prevent microbial proliferation. Different grades of water quality are required
depending on the route of administration of the pharmaceutical products. Other sources of guidance about
different grades of water can be found in pharmacopoeias and related documents.

In water laboratory three types of analysis are being conducted which are as follows:

 Physical Analysis

 Chemical Analysis

 Physio-chemical Analysis

PHYSICAL ANALYSIS

These include processes where no gross chemical or biological changes are carried out and strictly
physical phenomena are used to improve or treat the water. Examples would be coarse screening to
remove larger entrained objects and sedimentation (or clarification).

a) Coagulation and flocculation: One of the first steps in a conventional water purification process is the
addition of chemicals to assist in the removal of particles suspended in water. Particles can be inorganic
such as clay and silt or organic such as algae, bacteria, viruses, protozoa and natural organic matter.
Inorganic and organic particles contribute to the turbidity and color of water. The addition of inorganic

25
coagulants such as aluminum sulfate (or alum) or iron (III) salts such as iron (III) chloride cause several
simultaneous chemical and physical interactions on and among the particles. Within seconds, negative
charges on the particles are neutralized by inorganic coagulants. Also within seconds, metal hydroxide
precipitates of the aluminum and iron (III) ions begin to form. These precipitates combine into larger
particles under natural processes such as Brownian motion and through induced mixing which is
sometimes referred to as flocculation. The term most often used for the amorphous metal hydroxides is
"floc." Large, amorphous aluminum and iron (III) hydroxides adsorb and enmesh particles in
sedimentation and filtration.

b) Sedimentation: In the process of sedimentation, physical phenomena relating to the settling of solids
by gravity are allowed to operate. Usually this consists of simply holding the water for a short period of
time in a tank under quiescent conditions, allowing the heavier solids to settle, and removing the
"clarified" effluent. Waters exiting the flocculation basin may enter the sedimentation basin, also called a
clarifier or settling basin. It is a large tank with low water velocities, allowing floc to settle to the bottom.
The sedimentation basin is best located close to the flocculation basin so the transit between the two
processes does not permit settlement or floc break up. Sedimentation basins may be rectangular, where
water flows from end to end or circular where flow is from the centre outward.

c) Aeration: Another physical treatment process consists of aeration- that is, physically adding air,
usually to provide oxygen to the water.

d) Filtration: After separating most floc, the water is filtered as the final step to remove remaining
suspended particles and unsettled floc. Rapid sand filters: The most common type of filter is a rapid sand
filter. Water moves vertically through sand which often has a layer of activated carbon or anthracite coal
above the sand. The top layer removes organic compounds, which contribute to taste and odor. The space
between sand particles is larger than the smallest suspended particles, so simple filtration is not enough.
Most particles pass through surface layers but are trapped in pore spaces or adhere to sand particles.
Effective filtration extends into the depth of the filter. This property of the filter is key to its operation: if
the top layer of sand were to block all the particles, the filter would quickly clog. Some water treatment
plants employ pressure filters. These works on the same principle as rapid gravity filters, differing in that
the filter medium is enclosed in a steel vessel and the water is forced through it under pressure.

Advantages: Filters out much smaller particles than paper and sand filters can. Filters out virtually all
particles larger than their specified pore sizes. They are quite thin and so liquids flow through them fairly
rapidly. They are reasonably strong and so can withstand pressure differences across them of typically 2-5
atmospheres. They can be cleaned (back flushed) and reused Slow sand filters Slow sand filters may be
used where there is sufficient land and space, as the water must be passed very slowly through the filters.
The filters are carefully constructed using graded layers of sand, with the coarsest sand, along with some
gravel, at the bottom and finest sand at the top. Drains at the base convey treated water away for
disinfection. Filtration depends on the development of a thin biological layer, called the zoogleal layer or
Schmutzdecke, on the surface of the filter. Membrane filtration Membrane filters are widely used for
filtering both drinking water and sewage. For drinking water, membrane filters can remove virtually all
particles larger than 0.2 um-including giardia and cryptosporidium.

CHEMICAL ANALYSIS

It consists of using some chemical reaction or reactions to improve the water quality. Probably the most
commonly used chemical process is chlorination.

26
a) Chlorination: The most common disinfection method involves some form of chlorine or its
compounds such as chloramine or chlorine dioxide. Chlorine is a strong oxidant that rapidly kills many
harmful micro-organisms. Because chlorine is a toxic gas, there is a danger of a release associated with its
use. This problem is avoided by the use of sodium hypochlorite, which is a relatively inexpensive solution
that releases free chlorine when dissolved in water. Chlorine solutions can be generated on site by
electrolyzing common salt solutions. A solid form, calcium hypochlorite, releases chlorine on contact
with water.

b) Ozone disinfection: Ozone is an unstable molecule which readily gives up one atom of oxygen
providing a powerful oxidizing agent which is toxic to most waterborne organisms. It is an effective
method to inactivate harmful protozoa that form cysts. It also works well against almost all other
pathogens. Ozone is made by passing oxygen through ultraviolet light or a "cold" electrical discharge.
Some of the advantages of ozone include the production of fewer dangerous by-products and the absence
of taste and odour problems. Another advantage of ozone is that it leaves no residual disinfectant in the
water.

c) Neutralization: A chemical process commonly used in many industrial water treatment operations is
neutralization. Neutralization consists of the addition of acid or base to adjust pH levels back to
neutrality. Since lime is a base it is sometimes used in the neutralization of acid wastes.

d) Coagulation: Coagulation consists of the addition of a chemical that, through a chemical reaction,
forms an insoluble end product that serves to remove substances from the wastewater. Polyvalent metals
are commonly used as coagulating chemicals in water treatment and typical coagulants would include
lime (that can also be used in neutralization), certain iron containing compounds (such as ferric chloride
or ferric sulfate) and alum (aluminum sulfate)

Fig 4.1

27
Fig 4.2: Tuyil pharmaceutical industry water treatment lab.

4.1 Biological treatment methods

This method uses microorganisms, mostly bacteria, in the biochemical decomposition of wastewaters to
stable end products. Generally, biological treatment methods can be divided into aerobic and anaerobic
methods, based on availability of dissolved oxygen.

The solids which are removed during treatment are primarily organic but may also include
inorganic solids. Treatment must also be provided for the solids and liquids which are removed as sludge.
Finally, treatment to control odors, to retard biological activity, or destroy pathogenic organisms may also
be needed. While the devices used in wastewater treatment are numerous and will probably combine
physical, chemical and biological methods, they may all be generally grouped under six methods:

1. Preliminary Treatment

2. Primary Treatment

3. Secondary Treatment

4. Disinfection

5. Sludge Treatment

6. Tertiary Treatment Preliminary Treatment:

At most plants, preliminary treatment is used to protect pumping equipment and facilitate subsequent
treatment processes. Preliminary devices are designed to remove or cut up the larger suspended and

28
floating solids, to remove the heavy inorganic solids, and to remove excessive amounts of oils or greases.
To affect the objectives of preliminary treatment, the following devices are commonly used:

1. Screens rack, bar or fine

2. Comminuting devices -- grinders, cutters, shredders

3. Grit chambers

4. Pre-aeration tanks

In addition to the above, chlorination may be used in preliminary treatment. Since chlorination may
be used at all stages in treatment, it is considered to be a method by itself. Primary Treatment In this
treatment, most of the settleable solids are separated or removed from the wastewater by the physical
process of sedimentation. When certain chemicals are used with primary sedimentation tanks, some of the
colloidal solids are also removed. The primary devices may consist of settling tanks, clarifiers or
sedimentation tanks. Because of variations in design, operation, and application, settling tanks can be
divided into four general groups:

1. Septic tanks

2. Two story tanks -- Imhoff and several proprietary or patented units

3. Plain sedimentation tank with mechanical sludge removal

4. Upward flow clarifiers with mechanical sludge removal When chemicals are used, other auxiliary
units are employed. These are:

a. Chemical feed units

b. Mixing devices

c. Flocculators

SECONDARY TREATMENT

Secondary treatment depends primarily upon aerobic organisms which biochemically decompose
the organic solids to inorganic or stable organic solids. The devices used in secondary treatment may be
divided into four groups:

1. Trickling filters with secondary settling tanks

2. Activated sludge and modifications with final settling tanks

3. Intermittent sand filters

4. Stabilization ponds

Chlorination: This is a method of treatment which has been employed for many purposes in all stages in
wastewater treatment, and even prior to preliminary treatment. It involves the application of chlorine to
the wastewater for the following purposes:

29
1. Disinfection or destruction of pathogenic organisms

2. Prevention of wastewater decomposition

A. odor control

B. Protection of plant structure

3. Aid in plant operation -

A. Sedimentation,

B. Trickling filters,

C. Activated sludge bulking

4. Reduction or delay of biochemical oxygen demand (BOD)

Fig 4.3

30
4.2 DETERMINATION OF HARDNESS OF WATER

Natural water always contains a variety of dissolved ions, including Na + K+, Ca2+, Mg2+, CI-. HCO3-, and
some other. If concentrations of Ca and Mg ions are relatively large, the water is called hard.

Hard water may cause many problem. Therefore, it is important to have a simple method to
determine hardness. Such method is based on a titration of the water sample with a solution of a
complexing agent, named ethylene diamante tetra-acetate (EDTA).

4.3 THE DETERMINATION OF HARDNESS PROCESS

The sample (W1) was placed in a conical flask and if necessary, The sample was dilute with
distilled water to 100 ml. 5ml buffer solution was added, 5 ml triethanolamine solution, 5 ml magnesium
EDTA solution, and a sufficient amount of indicator was also added, the solution should have a clear
color. The solution was Mixed after each addition and The solution was Titrated with Na₂EDTA solution
until the blue, respectively green color, does not change (volume used = V1).

4.4 DETERMINATION OF CALCIUM

The analysis sample (W2) was placed in a conical flask and, It was diluted with distilled water to 100 ml.
5mL triethanolamine solution was added, 4 ml potassium hydroxide solution was also added, and after 5
minutes, a sufficient amount of indicator, so that the solution is clearly colored red or violet. The solution
was Mixed after each addition. The solution was Titrated with Na, EDTA solution until, the blue color
does not change (volume used = V2).

The total hardness can be calculated using the equation below

Ht-1000Vc/W

Which:

Ht is the total hardness, in mmol/L;

V1 is the amount of Na2EDTA solution used during the determination of hardness in ml;

c is the molar concentration of the Na2EDTA solution (cl resp. c'1), in mol/L;

W1 is the amount of water used for the determination of hardness, in ml.

The calcium ion content can be calculated using the Equation below

Ca=1000 V c/W

In which:

Ca is the calcium ion content, in mmol/L;

V is the amount of Na2EDTA solution used during the c is the molar concentration of die Na 2EDTA
solution (cl resp. c'1), in mol/L;

W2 is the amount of water used for determination of calcium, in ml.

Calculate the magnesium ion content

31
2+=-2+Mgt Ca CHC in which: 2+ Mg

C is the magnesium ion content, in mmol/L.

For the conversion of calcium, respectively magnesium content of mmol/L to meq/L, the following
applies:

1 mmol calcium = 2 mq calcium 40.08 mg

1 mmol magnesium = 2 mq magnesium = 24.32mg.

4.5 PREVENTION OF INTERFERENCE

If the water contains more than 10 mg carbonate and/or hydrogen carbonate ions per liter, remove the
interfering amounts by acidification, by boiling for a short time and by neutralizing again on methyl red.
If the analysis sample contains more than 1.5 mg iron ions, then the amount of triethanolamine solution
added is not sufficient to stop the interference. In that case, per 2 mg iron ions, add another 5 ml
triethanolamine solution.

32
 SECTION FIVE

5.1. CONCLUSION

My SIWES program exposed me to the norms of my career, it gave me an opportunity to make use and
operate some laboratory apparatus and equipment's I was not exposed to before the program. SIWES
experience was really an educative experience and I am grateful for the privilege. I was able to gain
working experience and exposure like performing in-process checks and test analysis of the raw materials
and the drugs being manufactured in the factory and also oversee the production processes to ensure the
quality of the products conform with the lay down standard for it according the pharmacopeia. From
which I was able to understand more of the practical aspect of chemistry and gain expertise in handling
laboratory equipment. This training also builds my confidence in the knowledge of chemistry.

5.2. RECOMMENDATION

I recommend that the ITF board of trustee should generate a way of providing transport fare monthly for
student sent on SIWES as this was a great challenge for majority of us. I also recommend Tuyil
Pharmaceutical Industry as a very conducive environment for students to learn because it provides an
enabling environment with well-equipped laboratories, a better staff- student communication

5.3 ACHIEVEMENT AND OUTCOME OF SIWES

The laboratory is simply arrayed in such a way for easy experiments to be carried out; also for research
hypothesis. Scientist that are carrying out experiments always wear laboratory coat in order to avoid
accidents. The industrial training period that lasted for six months gave me the opportunity to be
acquainted with the laboratory equipment's, their standard operating procedure and principle of various
and how a qualitative and standard laboratory is supposed to operate.

33
 REFERENCE

Industrial Training fund (2008); Students Industrial Work Experience scheme (http://www.itf-
nigeria.com)

Tuyil handbook "Brief history of Tuyil pharmaceutical industry""

Harper's illustrated chemistry twenty-sixth edition-Robert K. Murray, Danryl K. Granner, Joe C. Davis,
Peter A Mayes, Victor W. Rofwell, Phd.

Wikipedia "production equipment diagrams"

Tuyil Standard laboratory Pharmacopeia

Ankur, C. (2016). Line Clearance In Pharmaceuticals Science article. 75(15), 1

Banks, P. (2010). Multiplexed Assays in the Life Sciences, Biotek Instruments Inc, 76(3), 477.

Dennis, A. (2007). What the call center industry can learn from manufacturing. Journal of Business,
54(5), 13.

Douglas, H. (2016). Assay. Online Etymology Dictionary 2016, Retrieved 13 Aug 2016, from
http//www.etymonline.com/&sa/Assay.html

Gray, J. R. (2004). Conductivity Analyzers and Their Application.Environmental instrumentation and

analysis journal, 54(4), 23.

Jakoby, W.B., and Ziegler, D. M. (1990). The enzymes detoxification../ Biol Chem, 99(15), 47-51

Kevin, R. (2003). GLPs and the importance of standard operating procedures BioPharm International,
16(8), 89.

Symon, K. (1971). Mechanics (pp.78). Belmonth CA: Addison-Wesley

34