Chapter one

1.1 Introduction

The student industrial work experience scheme (SIWES) which started in

Nigeria in 1973 is an accepted skill training program which forms part of the

approved minimum academic standard in the various degree programs for all

Nigerian Universities. It is aimed basically is to expose students to work

methods and techniques in handling equipment and Machinery that may not

be available in the Universities and also to provide student with an

opportunity to apply their theoretical knowledge in real work situations

thereby bridging the gap between university work and actual practices.

The Student Industrial Work Experience Scheme started in 1974 with the

establishment of the ITF in 1971. During the formative years, ITF solely

funded the scheme. As the financial burden became too heavy and

unbearable to ITF, it withdrew from the scheme in 1978. The programme

was then handed over to both the National Universities Commission (NUC)

and the National Board for Technical Education (NBTE) in 1979. By

November 1984, the Federal Government reverted the management and

implementation of SIWES to ITF and completely took over the burden of

funding the programme. To give legal backing to the SIWES, Decree 16 of

1984 was enacted. Part of the provisions of the decree states that; “All

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students of specialized engineering, technology, business, applied science or

applied art programmes in higher institution shall be required to have a

compulsory supervised industrial attachment as part of their regular studies

in such a manner as may be prescribed by their boards or commission”.

1.1 Objectives of SIWES

1. To acquaint students with the relevant skills, knowledge, ethics and

experience required of students in the career of science laboratory

technology practice.

2. To avail students the opportunity of handling and maintaining of various

laboratory equipment for perfect transformation of scientific knowledge

or hypothesis already acquired into practical reality which must be

accurate dependable and verifiable for the benefits of mankind.

3. To abreast students with how to observe various safety rules and

maintenance culture.

4. To learn how to imbibe the good culture of keeping daily records of

scientific and technological events.

5. To acquire the technicality of writing standard practical reports and

reports of any kind.

6. To enable students build their confidence in the chosen career.

7. To serve as a veritable avenue for clear in depth understanding of the

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 course which consequentially improves academic performance?

8. To improve students communication and interpersonal skills.

9. To involve employers of labour in joining the learning institution sector

to train and graduate qualified personnel.

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 CHAPTER TWO

2.1 Company profile

Britex Nigeria Limited is a private limited liability company incorporated on

18th July 2011 in Nigeria under CAMA. However, it commenced pre-

incorporation business on 1st of February 1999 with just the managing

director Dr. Okei C. Friday as a chemical company and consulting firm. The

company has offices in the following locations, 16 Obi Wkali Street,

Rumuekini , Port Harcourt , Rivers state and 54 summit road (Jondora plaza)

opposite old state Secretariat, Asaba, Delta State, Nigeria.

Over these years the company has maintained its integrity in the sales and

marketing of genuine, high quality, fine and industrial chemicals, active

ingredient, fragrances and specialty raw materials. Consequently NAFDAC

enlisted the company as one of the marketing companies; for the marketing

of chemicals in Nigeria.

The company achieved another great feat in 2005 by establishing a public

analyst/analytical laboratory in line with IPAN decree 100 of 1992 for the

analysis of water, food, cosmetics, herbal remedies, medical devices,

polyurethane materials etc .the analytical laboratory has the wet chemistry,

instrumentation and microbiology sections. Also the laboratory is equipped

with modern analytical equipment and relevant test methods/standards. The

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laboratory currently carries out a lot of collaboratives research and Analysis

with SON, NAFDAC, EPC and several higher institutions, manufacturing

companies and students across the country.

The company has developed products for over 200 companies and has

assisted them in registering over 1000 products with NAFDAC and SON.

The company has retainership arrangement with several corporate

organizations for man power training and development in analytical

procedures, good manufacturing practice (cGMP), fumigation/pest control

services and water treatment plant installation/monitoring.

2.2 Company vision statement

i. To be one of the foremost in the provision of excellent, professional

scientific analytical services in Nigeria and beyond.

2.3 Company mission statement

i. To adopt the best scientific analytical practices in service delivery by

improving, promoting industrial development In Nigerian and beyond.

2.4 Organogram of the Company

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CHAPTER THREE

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3.1 Knowledge acquisition and skill development

Knowledge acquisition refers to the knowledge that a firm can try to obtain

from external sources. External knowledge sources are important and one

should therefore take a holistic view of the value chain. The knowledge

acquisition component allows the expert to enter their knowledge or

expertise into the expert system, and to refine it later as and when required.

The knowledge acquisition process is usually comprised of three principal

stages:

1. Knowledge elicitation is the interaction between the expert and the

knowledge program to elicit the expert knowledge in some systematic

way.

2. The knowledge thus obtained is usually stored in some form of human

friendly intermediate representation.

3. The intermediate representation of the knowledge is then compiled into

an executable form (e.g. production rules) that the inference engine can

process.

The chapter entails the skill and knowledge acquired during the course

of the trainee attachment (3 months). In course of the training the trainee

was exposed to various laboratory skills as regard analytical work carried

out in the laboratory and in the course of the skills lots of knowledge was

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gained by the trainee. The trainee was also exposed to various apparatus and

equipment used in the laboratory for various work.

3.2 High Performance Liquid Chromatography

The high performance liquid chromatographic machine is an instrument that

is basically used in carrying out identification test (qualitative analysis) and

chemical assay test (quantitative analysis) of drugs sample in comparison

with that of a known standard.

3.3 Essential Components of HPLC Machine

a. The Bottles: There are four (4) bottles on the HPLC machine labeled A-

D each of the bottles has tubes connected to other parts of the machine.

The tubes run into the degasser. The bottles are used in running the

machine to carry out the test. Thus the bottles contained the mobile

phase.

b. The Degasser: This component helps to remove air bottles that is coming

from the solvent in bottles.

c. Quantenary Pumps: The pumps samples the mobile phase through the

injector port i.e. the degassed solvent coming from the degasser is

channel by the quaternary pumps to the injectors port where it collects

the samples to be analysed to the colume. Also present here is the punch

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 valve that helps to further degas the solvent if the degasser does not

achieve optimum degassing.

d. The Column: This is where the actual separation takes place. It is a long

tube that is peaked higly with silical gel.

e. Variable Wavelength Detector: This component detects the sample at a

specific wavelength using ultraviolet light.

f. Injector Port: This is the component in which the sample to be analyzed

is injected.

NB: Quantification uses peaks Area or Height to determine the

concentration of the component in the sample.

Principle

This machine works with the principle of separation technique where the

solutions are separated by eluting the various component of the solution at

different times in form of identifiable peaks.

3.4 Spectrophotometer

The spectrophotometer is an instrument that is used in analytical chemistry

and biochemistry for qualitative analysis (chemical Assay test) and for

qualitative analysis (Identification test). These compounds maybe identified

by their characteristics absorption spectra in the ultraviolet, visible or infra-

red.

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3.4.1 Essential Components of the Spectrophotometer

a. Light source.

b. Collimator: This is a focusing device that directs light to a particular

body.

c. Monochromator: This device splits into different wavelength.

d. Wavelength Selector or Slit: This component select wavelength.

e. Cuvette: This is the container in which the sample in whose

concentration is to be determined is place and the blank.

f. Photocell: The photocell detects the sample in the solution and makes its

possible for the meter to read.

3.4.2 Principle behind the Spectrophotometer

The spectrometer works with the principle of light ray passing through a

medium. When this ray of light (monochromatic light) of initial intensity I o

passes through a solution in a transparent vessel. Some of the light is

absorbed so that the intensity of the transmitted light I is less than Io i.e. the

initial intensity is more than the final intensity.

The relationship between I and Io depends on the path length of the

absorbing medium (L) and the concentration of the absorbing medium.

Hence the principle behind the spectrophotometer follows the BEER-

LAMBERT’S LAW which states that the absorbance of a given solution

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passing through a transparent medium is directly proportion to the

concentration © of the medium and the length of the light path (L).

Hence from Beer-Lambert’s Law.

Where

A = The absorbance

C = The concentration of the solution

L = Length of light path.

Note: Length of light path is usually fixed (1cm)

3.5Facilities and equipment in the laboratory

The facilities and equipment found in the laboratory are of various class

ranging from protective equipment which include; lab coat, goggles, hand

gloves, nose mask to analytical equipment and machines under these

category we have various equipment use for analytical work like the

incubator, autoclave, microscope, beam balance, refrigerator etc and also

glass wares used in the course of an analysis/experiment lastly we have the

maintenance/safety tools which include the fume cupboard, fume extraction

unit, fire extinguisher etc these various equipment are very useful and are

readily available in the laboratory for the safety running of the laboratory

during and off duty.

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Figure 2: Electronic balance Figure 3: Beakers

Figure 4: Analytical balance Figure 5: Refractometer

Figure 6: Spectrophotometer Figure 7: Thermometer

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Beakers: It is a simple container used for storing, mixing and heating

liquids, it is cylindrical in shape, with a flat bottom and a small spout to aid

pouring.

Test tube: It is used to handle chemical it consist of a finger – like length of

glass and a rounded U – shaped bottom

Test tube rack: It is used to hold upright multiple test tube at the same time,

it provide support and helps in organizing of test tube.

Glass stirring rod: It is also known as stirring rod. It is used to mix

chemical and liquids.

Measuring cylinders: It is used to measure the volume of liquids. It consists

of a narrow cylindrical shape and marked line on the graduated cylinder.

Pipette: It is used to transport a measured volume of liquid.

Burette: It is used for the dispensing of variable measured amounts of

chemical solution. It consist of a stop cork or a control flow a volume

marking and a tip.

3.5 Safe working practices in the laboratory

Safety is of paramount when working in the laboratory as it helps to limit the

level of accident and hazards in the laboratory, these safety measures include

the following;

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1. Always keep your laboratory clean and make sure the gang ways are

always free from obstruction.

2. Experiments involving emission of obnoxious gases or vapours should be

carried out in fume cupboards.

3. Always empty all dustbins in the lab at least once a day. Ensure to throw

different wastes in their appropriate bins to avoid unwanted reaction in

the same dust bin.

4. Always place chemicals, apparatus and equipment in their appropriate

storage space when not in use.

5. Never leave supporters or covers of containers of chemicals especially

concentrated lying about on the bench tops or shelves. Thus, always

stopper back any used bottle of chemicals immediately after use to avoid

mixing up of cover or stoppers.

6. Firefighting equipment must be readily available and accessible.

7. Gas pipelines should be regularly checked for leakage with soapy water

only whole gas cylinder should be stored upright preferably in outside

stores.

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3.6 Specific work done

3.6.1 Preparation of solution

Solutions are often used in the laboratory for various chemical analysis and

these solutions are prepared in various concentrations either in molarity,

normality or percentages. Solutions are prepared in molarity are referred to

as molar solution and while those prepared in normality are normal solutions

and these are used in carrying out precise analytical analysis. Solution when

prepared in percentage can either be in weight per volume (w/v) or volume

per volume (v/v) or percentage.

Molarity (M): The Molarity of a solution is the number of moles of solute

contained in 1000 ml of a solution. Since the equivalent weight varies with

the reaction involved, ambiguity can be avoided by expressing

concentrations in terms of molar solution, when equivalent of a substance is

the same as the molecular weight, then a molar solution is identical with a

normal solution and they are expressed in mole (e.g. 1M, 0.5M).

Normality (N): The normality of a solution is a solution which contains one

gram of equivalent weight of a substance in 1000 ml of solution. The gram

equivalent of a compound depends upon the reaction which it undergoes,

solution prepared in normality are expressed in normal (e.g. 1N).

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Percentage (%): Percentage solution is an approximate solution and are

usually expressed in percent by weight, it can be said to be a number of

grams of a solute dissolved per 100 ml of solution.

N.B: In the preparation of solution it is advisable to prepare the solution

using distill water to avoid contamination

Preparation OF 0.1M Sodium Hydroxide (NaOH)

Apparatus: Measuring cylinder, beaker, volumetric flask, spatula

Reagent: Distilled water, NaOH (AR)

Method: Exactly 20 g of NaOH was weighed using a weighing balance and

then dissolved in a little volume of distilled water in a beaker on dissolution

was transferred into a 1000 ml volumetric flask and then made up to mark

with distilled water.

3.6.2 Standardization of solution

Standardization is carried out in other to ascertain the concentration of

solutions prepared before they are used to carry out chemical analysis. In the

course of standardizing a primary standard of known concentration is titrated

against the solution to be standardized which is the secondary standard.

Primary Standard: It is the solution that the strength is known and the

concentration cannot deteriorate with time. e.g. H 2SO4, Iodine, HCl, arsenic

trioxide, KMnO4, oxalic acid.

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Secondary standard: These are solutions that tend to loses their strength

with time using such solution requires one to standard the solution using a

primary standard. e.g. NaOH, Na2CO3.

On titrating the factor is calculated and this is defined as the milliliters of

actual strength which is equivalent to 1 m of solution of normal strength, this

is calculated using the formula below;

The value of the factor should be within the range of 0.9 – 1 to know

if the strength of solution is standard.

Standardization of 1M NaOH Using Sulphamic Acid

Principle: Sulphamic acid, H2NSO3H, may be obtained in crystalline form

99.9% purity. The crystals are of constant composition and thus suitable as a

primary standard. The acid has one replaceable hydrogen and titrates as a

strong monobasic acid. It undergoes slow hydrolysis in aqueous solution.

H2NSO3H + H2O → NHaSO4 + H+

Apparatus: Analytical balance, spatula, beaker, burette, pipette, dropper,

glass stirring rod, conical flask

Reagent: NaOH, sulphamic acid, methyl orange, phenolphthalein, distill

water, water heating mantle

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Method: About 3 g of sulphamic acid was weighed and dissolved in about

50 ml of distilled water which stands as the secondary standard. The mixture

was titrated with a prepared 1M NaOH solution provided in the burette

standing as the primary standard methyl orange (2 drops) was used as the

indicator. The end point is the appearance of a deep orange colour just prior

to full yellow colour. The procedure was repeated twice and average was

calculated. Three further titrations were carried out using phenolphthalein as

indicator (5 – 10 drops). The end – point is the first pink colour to persist for

15 seconds. Vigorous shaking was avoided as this causes CO 2 from the

atmosphere to discharge the colour prematurely. Again the average result

was also calculated. The methyl orange and the phenolphthalein factors of

the approximately 1M NaOH were then calculated.

3.6.3 Method of extraction of active ingredient

There are several methods used to extract active ingredient from plants

extraction of oil from seeds, amongst these methods are

1. Cold maceration method

2. Soxhlet extractor

3. Percolation method

Cold Maceration Method: The plant was soaked in a suitable solvent either

water or ethanol at 20°C for 3 days then sieved to get the liquid active

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ingredient. The method was used to extract the active ingredient from lemon

grass, bitter leaf, etc.

Soxhlet Extraction: The sample was poured into the thimble the suitable

solvent which can be ethanol, methanol etc was poured into the dual purpose

flask, the whole setup was connected to a condenser which was connected to

inlet and outlet pipe, On heating, the solvent extract the active ingredient

from the sample, the condenser takes the vapour back to the dual purpose

flask (receiving flask). The process continues until the solvent in the sample

turn colourless. The extracted solvent is taken to the drying oven to dry.

Percolation Method of Extraction: This method was done by heating the

sample with a suitable solvent which can be water or ethanol, allowed to boil

then mill out the juice which bond with the active ingredient.

Rotary Evaporator

Rotary evaporator is a device used for the efficient and gentle removal of

solvents from sample by evaporation under pressure. It consist of a

condenser, receiver flask an external vacuum pump, distillation flask and the

water bath.

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3.6.4 Phytochemical screening

Phytochemical screening was carried out on a leave extract, extracted using

soxhlet extraction method, below are the various test carried out and their

procedure;

Test for Taninns:Few drops of 0.1% ferric chloride was added to 1ml of

extract and a green or a blue – black coloration was observed which

confirms the presence of tannin.

Test for Saponin:2ml of the extracts was reacted with 3ml of distilled water

and shaken vigorously for a stable persistent froth. The frothing was mixed

with 3 drops of olive oil and shaken vigorously, then observed for the

formation of emulsion which confirms a positive presence of Saponin.

Test of Flavonoids: About 2ml of extracts was treated with few drops of

10% sodium hydroxide solution formation of intense yellow colour, which

becomes colourless on addition of dilute hydrochloric acid, indicates the

presence of flavonoids.

Test for Steroids:2ml of acetic anhydride was added to 2ml extract of each

sample followed by careful addition of 2ml H 2SO4. The colour changed from

violet to blue or green indicate the presence of steroids.

Test for Terpenoids (Salkowski test):Two ml (2ml) of each extract was

mixed with 2ml of chloroform, and 2ml concentrated H 2SO4 was carefully

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added to form a layer. A reddish brown coloration at the interface was

formed to show positive results for the presence of terpenoids.

Test for Cardiac Glycosides (Keller – Killani test): Two ml of each

extracts was treated with 2ml of glacial acetic acid containing one drop of

ferric chloride solution. This was underplayed with 1ml of concentrated

sulphuric acid. A brown ring at the interface indicates deoxysugar

characteristics of cardenolides. A violet-green ring appearing below the

brown ring, in the acetic acid layer, indicates the positive presence of

glycoside.

Test for Alkaloids:2ml of the extract was stirred with 2ml of 1% aqueous

HCl on a steam bath and filtered while hot. Distilled water was added to the

residue and 1ml of the filtrate was treated with a few drops of either Mayer’s

reagent (Potassium mercuric iodide- solution) or Wagner’s reagent (solution

of iodine in Potassium iodide) or Dragendorff’s reagent (solution of

Potassium bismuth iodide). The formation of a cream colour with Mayer’s

reagent and reddish-brown precipitate with Wagner’s and Dragendorff’s

reagent give a positive test for alkaloids.

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Secondary metabolites Observation Inference
Tannins Blue black colour Present
Saponnins Persistent forming Present
Alkaloids Faint cream colour Suspected
Flavonoids Red colour Absent
Cardiac glycoside Red ring at the interface Present
Steroids Green colour Present
Terpenoids Reddsh brown at the present
interface

3.7 Column chromatography

Chromatography, which owes its rapid growth during the past three decades

to its speed, simplicity, relatively low cost and wide applicability as a

separation tool, is one of the most valuable techniques for the separation,

isolation, purification and identification of organic compounds from simple

or complex mixtures. In column chromatography adsorbents used generally

include alumina (anhydrous or with 7 or 4% water, basic neutral or

deactivated) carboxymethylcellulose, kieselguhr and silica gel. The progress

of separation is usually monitored by TLC the capillary action of solvent use

for extraction and the solvent in the TLC tank. The eluting powers of various

solvents, i.e. their ability to remove a given substance down a column are

generally found to occur in the following order: alkanes, carbon

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tetrachloride, toluene dichloromethane, chloroform, diethyl ether, ethyl

acetate, acetone, ethanol, methanol and water. In the case of using three (3)

or more different solvents for extraction, the least polar solvent is allowed to

extract first before others.

Method: The column was first packed with silica gel of mash size 60 – 120

and then a ball of cotton wool inserted into the column on this the sample

extract was placed and solvent which served as the mobile phase (methanol,

n-hexane and chloroform) were introduced into the column starting with the

least polar solvent, on elucidating the fractions were collected and rendered

to phytochemical screening and check for the metabolite present the ones

with sample metabolites were bucked together while those having more than

one constitute were tagged as not pure and then discarded, the pure fractions

were further sent for TLC analysis for ascertain its purity.

3.8 Quantification of alkaloid in plant sample

Apparatus: Beaker, what man filter paper, measuring cylinder, analytical

balance, conical flask

Reagent: Ethanol (10%), 10% acetic acid, conc. ammonia,

Method: Exactly 2.5 g of plant sample dried and grounded leaves was

weighed and 100 ml of 10% acetic acid in ethanol was added to the sample

placed in a conical flasks and it was allowed to stand for 4 hours after which

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it was filtered. About 50 ml of the filtrate was taken and heated to 25 ml and

25 ml of concentrated ammonia was added and precipitate was formed. The

precipitate was filtered, dried and weighed and the result gotten was

recorded. Then the amount of alkaloid present in the sample was then

calculated using the formula below;

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 CHAPTER FOUR

Conclusion and recommendation

4.1 Conclusion

The Students Industrial Work Experience Scheme (SIWES) is to give

students theprivilege to be exposed to training that is related to their course

of study. As a result ofthis scheme, students acquire more knowledge of

various kinds from their places oftraining.Conclusively, the purpose for

which this programme was created has indeed being achieved, knowledge

gained during the period of attachment will be of great use to me. I was

expose to various practical analysis carried out the laboratory and also

various laboratory ethic and safety measures in the laboratory.

4.2 Recommendation

The following recommendations were based on the problems and challenges

encountered during the course of the Student Industrial Work Experience

Scheme (SIWES) and as a solution to the identified problems.

Proper coordination and supervision of the exercise: The various bodies

involved in the management of the SIWES exercise i.e. Federal

Government, Industrial Training Fund (ITF), NUC, NBTE and NCCE

should come together and fashion out a modality that will ensure smooth

operation of the SIWES exercise. Efforts should be made to ensure that

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students attached to the organization are properly supervised to ensure that

what they are doing is in line with the objectives of the SIWES exercise.

Acceptance of students: The various bodies involved in the management of

the SIWESprogrammes should liaise with the various industries ahead of

tune so as to minimize or reduce to the barest minimum the high level of

refusal to accept students for their industrial training participation.

Financial support: The saying that money answers all things is not an

understatement because for every possible step, there should be enough

finance to achieve it. Finance always posed a lot challenges towards proper

enhancement of students during industrial training. As I earlier observed that

lack of finance hinders students from going to their place of work earlier or

going to the right place for development of knowledge in their field of study.

The establishment are expected to at least give the students transport fair

even thou they cannot pay them on monthly basis.

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