CHAPTER ONE

INTRODUCTION

1.1 SIWES and its Objectives

The Nigerian Industry depends on the technical competence of the manpower for the

operation and maintenance of equipment, plants and resources.

The students’ Industrial work Experience Scheme (SIWES) is the accepted skills training

programme, which forms part of the approved minimum academic standard in the various

degree programmes for all the Nigerian universities. The scheme bridges the gap existing

between theory and practice of the Engineering and technology, sciences, agriculture,

medical, environment sciences, technical and science education and other professional

work methods and ways of safeguarding the work areas and workers in industrial in other

organizations.

The objectives of the students’ industrial work Experience Scheme (SIWES) according to

the Industrial Training Fund (ITF) 2013 are to:

1) Provide an avenue for students in institutions of higher learning to acquire

industrial skills and experience in their courses of study.

2) Prepare students for the industrial work situations they are 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 easier, and enhance students

contacts for later job placement.

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5) Provide students with an opportunity to apply their knowledge in real work

situation thereby bridging the gap between theory and practice and

6) Enlist and strengthen employers involvement in the entire educational process and

prepare students for employment after graduation.

1.2 DESCRIPTION OF ORGANIZATION

I applied to the National Agency for Food and Drug Administration and Control

(NAFDAC) an agency under the ministry of health; I was engulfed and posted to do my

industrial training at the area laboratory in Borokiri Port Harcourt, Rivers State.

This brief essay is a report of the experience I had for six months at the National Agency

for Food and Drug Administration and Control (NAFDAC) area laboratory Port Harcourt,

Rivers State, where I did my industrial training.

1.3 FUNCTIONS OF NAFDAC

NAFDAC has various functions:

1) Regulate and control the importation, exportation, manufacture, advertisement,

distribution, sales and use of drugs, cosmetics, medical devices, bottled water and

chemicals.

2) Undertake appropriate investigation into the production premises and raw materials

for food, drugs, cosmetics, medical devices, bottled water and chemical and establish

a relevant quality assurance system, including certification of the production site and

of the regulated products.

3) Establish and maintain relevant laboratories or other institutions in strategic area of

Nigeria as may be necessary for the performance of its functions.

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1.4 ORGANIZATIONAL CHART OF NAFDAC

NAFDAC ORGANOGRAM

CHAPTER TWO

Nafdac Port Harcourt Area laboratory is a unit of the laboratory services directorates with

the responsibility of laboratory examination of mainly food and water.

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 CHAPTER TWO

All laboratories are designed for their unique analyses and are structured to accommodate

different staff with different positions of which the laboratory is headed by the head of lab.

The NAFDAC area laboratory is basically divided into four (4) departments or

laboratories as follows;

1) Sample reception unit/department

2) Food laboratory; which is divided into three section;

3) Food registration laboratory

4) Food compliance laboratory

5) Sea food laboratory

6) Water laboratory

7) Microbiology laboratory

1) Sample reception unit: The sample reception unit (SRM), is a part of the

laboratory that deals with receiving, registration and distribution of the samples

brought in by the established investigation department (EID) or Port Inspection

Directorate (PID).

All samples brought into this section must have a job order which contains the
following:

 Name of the sample

 Manufacturers name and address

 Batch No.

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  Manufactured and expiration date

 Receipt of payment of analysis

 Reason for analysis

After verifying samples for the above information, the sample is then given an ID number

in the format ‘PH/NAME OF LAB ANY PURPOSE/SERIAL NO/YEAR’. Which is used

to identify the sample (product). The samples (product) are distributed to their various

laboratory with a JOB card, which contains space for writing down the results for analysis

carried out on the product.

2.1 NAFDAC STANDARD OPERATING PROCEDURE (SOP)

The standard operating procedure (SOP) is designed for the unique analysis for different

laboratories and to make work easier for the analyst, interns and IT’s. The methods used in

analysis are strictly approved by NAFDAC and they are documented in the standard

operating procedure (SOP).

Using any other methods of analysis, other than the ones contained in the SOP is not

allowed and such result will not be accepted and validated.

Food laboratory: Is divided into three (3), the food registration, food compliance and the

sea food lab.

Food registration laboratory: This section handles locally made products, analysis are

been carried out to confirm the declared parameter. And to make sure that the

manufacturer claims is confirm to the limits of specification and standards for the purpose

registration.

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Food compliance laboratory: This section deals with mostly imported product, analyzed

for the purpose of compliance and standard.

Sea food laboratory: This laboratory deals with all kinds of sea foods such as frozen fish

and stock fish.

2.2 VARIOUS ANALYSIS CARRIED OUT IN THE FOOD LABORATORY

Title: Moisture content determination using the moisture analysis

Moisture is the amount of water in a product. Moisture content is carried out to determine

the percentage of water content and shelf life of the product.

Aim: To ensure that moisture content of the sample complies with its limit of

specification.

Principle: This method is based on loss on drying automatically at a temperature of 1050C

to determine the shelf life of a particular product.

Procedure:

 The instrument was switched on and allowed to warm up and stabilize for at least

10 minutes in order to reach the preset temperature in order to reach the preset

temperature of 050C.

 The sample chamber was opened and now dry platinum foil was placed on it.

 The prepared sample was spread to weight 2.0g on the pan.

 The sample chamber was closed and the dry programmer starts reading after

pressing the “enter key”.

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  The drying programmer shuts off automatically once no further moisture or weight

loss is detected.

 The % moisture loss was recorded as the moisture content value.

 The chamber was opened and the pan draft shield off loaded from the plan support.

Title: Ash Content Determination

Ash content determination involves the heating up of a food sample (product) at a very

high temperature removing the organic materials, while the inorganic materials remain.

Why do we ash: We ash to get the inorganic components which might be harmless to

human health.

Ashing is done in a muffle furnace.

Determining the ash content may be important for several reasons:

1) Microbial stability: High mineral contents are sometimes used to slow the growth

of certain micro-organisms.

2) Nutrition: Some minerals are essential to a good healthy diet (e.g calcium,

phosphorus and sodium) whereas others can be toxic (e.g lead, mercury, cadmium

and aluminum).

Apparatus: Crucible, furnace, hot plate, weighing balance, spartula.

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Procedure:

1. An empty dried crucible was weighted as W1.

2. 2g of sample was weighted with the crucible as W2.

3. Crucible was placed in the hot plate to pre-ash (30mins-1hr).

4. Crucible was transferred to the furnace and allowed to ash properly (12-24hrs) at

550C.

5. Crucible was removed from the furnace and transferred to the desiccator and allowed

to cool.

6. A new weight of ashed sample with crucible was taken as W3.

Calculation:

W3  W1 100
 x
W2 1

Title: Determination of Acidity in food sample

Food acidity affects the ability of micro-organism growing in food and also the flavor in

food.

The acidity of food and drinks determines if it will actually encourage or discourage the

growth of microbes and also if will be detrimental to human health.

Aim: To determine the acid value in a food sample.

Reagent: O.I.N. sodium hydroxide (NaoH), Bromothymol blue (for coloured sample)

phenolpthallin indicator for colourless.

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Apparatus: Beaker, measuring cylinder, burette, retort stand

Procedure:

 10ml of the sample was measured into a conical flask.

 Add 1ml or 3 drops of indicator (bromothymol for coloured samples and

phenolphthalein for colourless sample).

 Titrate against 0.1N Na0H in the burette until colour change appears.

 Take your titre reading

Calculation

Titre value 100

x
weight of sample 1

Title: Determination of milk solid Non-fat (MSNF)

Aim: To determine solid non-fat in liquid diary products.

Reagents: Phenolpthalein, indicator, formalin, O.I.N NaOH.

Apparatus: Conical flask, burette, retort stand, procedure:

Procedure:

1) 10ml of the sample was poured into the concial flask.

2) 1ml or 3drops of phenolphthalein was added into the flask.

3) 3ml of formalin was added into the flask.

4) Then, titrated against 0.1N NaOH and reading was taken.

5) The blank is prepared in the same procedure in the absence of the sample.

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Calculation:

MSNF value = (Tv of sample – Tv of Blank) 5.67

Title: Trace metal analysis

Some of the metals analysed in food samples are zinc (Zn), lead (pb), iron (fe), copper

(cu), cadmium (cd). Some of these metal are essential to maintain the metabolism of the

human body, but at higher concentrations, they can be poisonous and have a tendency of

bioaccumulation.

Aim: To ensure the metals found in food sample are in line to international food standard

and safety limits.

Apparatus: 100ml volumetric flask, filter paper, fund.

Reagent: 1% Nitric acid.

Procedure:

1) Dissolve the ash obtained from the determination of ash content with 1% Nitric acid

by pouring into a fund using filter paper in a 100ml volumetric flask up to 100ml

mark.

2) Determine the absorption rate using the atomic adsorption spectrophotometer giving

the result in mg/kg or mg/l.

Note: The absorption rate can also be determined using smart spectrometer. On the smart

spectrometer the result comes in PPM (parts per million). It is calculated this;

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 Concentration ( ppm) 100
x
weight of sample 1

Title: Rancidity in oil (KREIS-TEST)

Rancidity is the unpleasant odours and flovours in foods resulting from determination in

the fat or oil portion of the food.

Aim: To determine the extent of spoilage in oil and fat.

Principle: This is the natural process of decomposition of lipids by either oxidation or

hydrolysis and invariable the both. The ingestion of rancid lipids can cause the

development of many diseases including, cell membrane damage, neurodegeneraton

carcinogenesis, kidney and heart diseases.

Apparatus:

Test tube, beaker and measuring cylinder.

Reagents: 0.1% phloroglucinol solution, conc. Hydrochloric acid.

Procedure:

1. Measure 10ml of the oil or dissolved fat into a clean beaker.

2. Add 10ml each of 0.1% phloroglucinol solution and conc. HCL to the oil in the

beaker and mix thoroughly for 20 seconds.

3. A pink colour change indicates rancidity.

N/B: If V2 –V1 is greater than V2/2, the test is repeated using a similar amount of sample.

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Title: Determination of Potassium bromate in food

Potassium bromate (K2Bro2) is a compound which is used as an additive in food products

mainly bakery products. E.g bread. It functions as arising and softening agent in the dough

during baking, but has been banned because of its effect in human health (it is

carcinogenic).

Aim: To check the presence of potassium bromate in bread.

Apparatus: Petridish, measuring cylinder.

Reagent: 10% hydrochloric acid (HCL) 10% potassium iodide (KI).

Procedure:

i) Put some piece of bread in a petridish, and spread evenly.

ii) Takes equal volumes (10ml) of 10% HCL and 10% potassium iodide with a

measuring cylinder.

iii) Pour it on the bread in the petri-dish.

iv) Blue-black spots indicate presence of potassium bromate in the bread sample.

Title: Peroxide value:

Principle: The concentration of peroxides in an oil or fat gives an indication of the extent

of spoilage. This oil is treated with potassium iodide in an organic solvent. The peroxides

liberates the iodine from potassium iodide. The iodine is titrated with standard

thiosulphate.

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Purpose: Estimation of peroxide value (being a measure of degree of spoilage) in

oils/fats.

Scope: to ensure that the peroxide value of the fats or oils are within the limits of

specifications.

Apparatus: Boiling tube, water bath, titration flask, Burrette (25ml), short glass tube

(about 15cm in length).

Method: Lea’s volumetric method.

Reagents:

i) Potassium iodide

ii) Solvent mixture consisting 2 volume of glacial acetic acid and one volume of

chloroform (i.e 2:1).

iii) 5% potassium iodide solution.

iv) 0.002m sodium thiosulphate solution

v) Starch indicator

Procedure:

N/B: Test is carried out in subdued daylight.

i) Weight out 1g of oil or fat into a clean dry boiling tube.

ii) Add 1g powdered potassium iodide and 20ml solvent mixture.

iii) The tube was placed in boiling water bath for 60 seconds.

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iv) The content was transferred into a conical flask containing 20ml of 5% potassium

iodide solution.

v) Wash the tube twice with 25ml distilled water.

vi) Rinse a clean dry burette with 0.002m sodium thiosulphate solution and fill the

burette with the same solution to its zero mark and damp on a retortstand.

vii) Titrate the contents of the flask with 0.002m sodium thosulphate solution, using

starch as indicator towards the end point

viii) Record the title as V1.

ix) Carryout a blank determination that is minus the oil or fat.

x) Record the blank title as V2.

Calculation:

2(V1  V2 )
Peroxide value  M  q1kg
weight of sample

Title: determination of iodine value in oils and fats

Purpose: Estimation of the iodine value in oil and fats.

Method: Wij’s method

Scope: To ensure that the iodine value in fats and oils are within the limits of

specification.

Apparatus: 250ml glass stopper flat bottom flask, dropping pipette, piptte filter, 10ml,

15ml, 100ml bulb pipette, 25ml burette.

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Reagents:

1) Dissolve 16.5g iodine monochloride in glacial acetic acid and make up to 1-litre with

same solvent.

2) 10% potassium iodide solution

3) 0.1m sodium thiosulphate

4) Starch indicator

Procedure:

1. Weight about 0.2g to 0.5g of the oil of the oil or fat into a glass stopper flat bottom

flask of about 250ml capacity.

2. 10ml chloroform was added to the flask to dissolve the oil or fat.

3. 20ml of wij’s solution was added and covered with the already dampened stopper.

4. The solution was mixed and allowed to stand in the dark for 30 minutes.

5. 15ml of 10%% potassium iodide solution was added to the solution, 100ml of water

was added and mixed.

6. Three drops of starch indicator was added to the solution in the glass flask.

7. Rinse a clean dry burette with 0.1m sodium thiosulphate solution and fill the burette

with the solution to the zero mark.

8. Titrate the mixture in the flask with the standard thiosulphate solution, titrate until

you observe a dark pink colouration cleared in the dark, leaving a dense viscous pin

liquid to settle under the clear liquid.

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 (V1  V2 )
Iodine value (wij’s)  X 1.269
weight of sample

Title: Determination of acid value in oils and fats

Purpose: estimation of acid value (being a measure of the degree of spoilage) in oils and

fats.

Method: Titrimetric method

Scope: To ensure that the acid value of the fats or oils are within the limits of

specification.

Apparatus: 250ml conical flask, 25ml burette, retort stand, measuring cylinder 50ml.

Reagents:

1) Diethyl ether

2) 95% - 100% ethanol

3) Phenolphthalein indicator (1% Alcoholic solution)

4) 0.1M potassium hydroxide

Procedure:

1. Weight 5g of the oil or fat into a clean dry 250ml conical flask.

2. Into a 250ml conic mix 75ml diethyl ether with 75ml ethanol.

3. Add 1ml of phenolophthalein indicator solution.

4. Rinse a clean dry burette with 0.1m potassium hydroxide solution and fill the burette

with it to it’s zero mark and clamp to a retort stand.

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5. Neutralize the mixture of the diethyl ether and the ethanol with the 0.1m potassium

hydroxide.

6. Transfer 50ml of the neutralized mixture into the weighed oil or fat to dissolve it.

7. Titrate the dissolved oil or fat with o.1m potassium hydroxide solution from the

burette until you observe a light pink colour change.

8. Record your titre as Vml

Calculation:

(V x 5.61)
Acid value 
weight of sample

Also acid value = 2 x free fatty acid (FFA)

Title: Holde’s qualitative test for mineral oils in fats and vegetable oils

Purpose: To determine the presence of mineral oils in fats and vegetable oils.

Method: Qualitative method

Scope: To ensure that the fats or vegetable oils are within the limits of specification.

Apparatus: Two 50ml test tubes, water bath.

Reagents: 0.5m Alcoholic potassium hydroxide.

Procedure:

1) Weight 10ml of the method for or vegetable oil to the 50ml test tube.

2) Add 5ml of the 0.5m alcoholic potassium hydroxide.

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3) Heat on a boiling water bath with frequent agitation for some minutes to ensure

complete reaction.

4) To the not soap solution add water, 0.5ml at a time shaking and observing each

additional until 10ml has been add together.

5) The formation of turbidity indicates the presence of mineral oils.

Title: Monosodium glutamate (MSG) Test

Monosodium glutamate (MSG) is a flavor enhancer commonly added to seasonings.

Aim: To determine the amount of monosodium glutamate (MDG) in seasonings.

Apparatus: 100ml conical flask, measuring cylinder, 50ml beaker.

Reagents: 0.1m NaOH, bromothymol blue

Procedure:

 0.5g of the sample was weighed in to a 250ml volumetric flask.

 250ml of distilled water was then added.

 10ml of the ample was measured into a conical flask.

 Clean dry burette was rinsed with 0.1N NaOH solution.

 2 to 3 drops of bromothyomol blue (indicator) was added into the conical flask

containing the measured sample.

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 The sample was titrated with 0.1N NaOH to a blue end-point.

 The titre value was recorded as Tv

Calculation:

Tv x 14.7
% Glutamic acid  X 100
weight taken

% MSG = % Glutamic acid x 1.15

Where 1.15 is the factor for MSG

Value gotten must not exceed 1.15% max.

Title: Colour determination

Aim: TO determine the colour used in producing custard and wine product.

Different wine product and custard sample are added colour to make it look attractive and

presentable.

Examples of acceptable colours as caramel, sun set yellow etc.

Apparatus:

Beaker, knitty wool, busen burner, paper chromatatography, measuring cylinder, weighing

balance.

Reagent:10% NH3 and 0.1N NH3, conc Hcl, mobile phase(ethanol, isobutanol and water)

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Procedure:

 The knitty wool was sterilized by boiling in 10% NH3.

 The solution was boiled for about 10mins.

 The knitty wool was rinsed with distilled water.

 30ml of the sample was added ad boiled.

 While boiling, 2ml of conc Hcl was added and boiled for a while.

 The sample solution was poured out and rinsed again with distilled water.

 Little quantity of 0.1N NH3 was then added and heated to concentrate colour.

 A mobile phase made up of ethanol, isobutanol and water at ration 2:1:1 was

prepared.

 Sample colour was spites at the other end of the chromatorgraphic paper.

 The paper was placed in the mobile phase and left for some time.

Result:

The colour was confirmed if the standard colour travelled at the same rate in the mobile

phase.

Title: Determination of alcohol percentage

Aim: To determine the level of alcohol contain in the sample.

Apparatus: Heating mantle, volumetric flask, measuring cylinder, specific gravity bottle,

weighing balance, condenser.

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Reagents:

Distilled water, anti-bomb

Procedure:

i) 100ml of the sample was measured into a 500ml round bottom flask with a

measuring cylinder.

ii) 25ml of distilled water was added into the flask together with anti-foaming agents,

then the round bottom flask was placed on a heating mantle at 800C.

iii) And it was set up for distillation with 10ml of distilled water in a 100ml volumetric

flask.

iv) Then the alcohol was distilled into the 100ml volumetric flask to the 100ml mark

ready for specific gravity determination.

Specific gravity determination.

i) The empty specific gravity was weighed as W1.

ii) Then the specific gravity bottle was filled with water and weighed as W2.

iii) The distillate was then filled into the specific bottle and was weighed as W3.

Calculation:

w3  w1
Specific gravity 
w2 1

Title: Fat extraction

 Rose gottlieb’s method

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Aim: To determine the percentage of fat in food sample.

Apparatus: water bath, beaker, separating funnel, dessicator, oven.

Reagents: N-hexane or diethyl, ethanol, ammonia.

 Rose gottieb’s method is a gravimetric method used for determining fat is use

variety of food products, especially milk product.

This accelerated solvent extraction is another method that has been shown to be reliable

for the determination of fat concentration in milk.

Procedure:

1) A conical flask was dried in the oven, cooled in the desiccator and weighed as W1.

2) 5g of the sample was weighed into the beaker as W2.

 If the sample is solid, 10ml of distilled water must be added.

3) 2ml of concentrated NH2 (ammonia) was added into the beaker.

4) The beaker is heated in the water bath for 5mins and allowed to cool.

5) 10ml of concentrated ethanol was added into the beaker and the transferred to the

seperating funnel.

6) 50ml of N-hexane or diethyl ether was added and shaken continuously for 30

seconds and allowed to stand for 5mins.

7) The extraction was repeated three times using 50ml portion of either the solvents

(N-hexane or diethyl ether), the stopper was continuously moved each time to allow

the vapor escape.

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8) After allowing to stand for 5minutes for the third time, two layers are formed the

upper clear layer was then taken into the weighed conical flask.

9) The N-hexane or diethyl ether in the mixture was evaporated using hot water bath.

The residual oil was dried in an oven at 1500C to eliminate any moisture that might

be present.

10) It was then cool and weighed as W3.

Calculation:

w3  w1
1% fat 
w

(b) Soxhlet extraction method:

Aim: To determine the percentage fat in a solid food sample.

Apparatus: Soxhlet extractor, round bottom flask, heating mantle, weighing balance,

water bath, conical flask.

Reagents: N-hexane or petroleum ether.

Principle:
This involves the gravimetric (measurement by weight) estimation of fat from a dry

powdered solid after a continuous extraction with light organic solvent e.g N-hexane or

petroleum ether.

Procedure:
i) Dry and weight a conical flask as W1.

ii) 5g of the sample was weighed into a filter paper, wrapped and stapled.

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iii) Place the round bottom flask into the heating mantle and the extractor mounted on

the flask.

iv) The sample is dropped into the soxhlet extractor and 250ml of N-hexane or

petroleum ether was added into it.

v) Connect your flow and outflow of water into pipes to the extractor for effective

condensation.

vi) Then on your heating mantle to the highest (1000C) for maximum extraction for

1hour.

 The fat will be extracted into the round bottom flask leaving the residues in the

extractor.

vii) The extract and the N-hexane or petroleum ether in the flask are poured into the

weighed beaker and heated in the water bath for a few minutes to enhance the

evaporation of the solvent leaving the extracted fat.

viii) Then the beaker is cooled and weighed as W3

Calculation:

w3  w1
1% fat 
w2 x 100

Title: Determination of sugar content:

Sugar is the generic name for 5wet-tasting soluble carbohydrates, many of which are used

in food. Various types of sugar are derived from different sources. E.g sucrose (known a

table sugar) is derived from sugar cane and sugar beet.

This analysis has 2 phases.

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a) Determination of Reducing sugar

Aim: To ensure that the sugar content in food sample are within the limit of the

specification.

 A reducing sugar is any sugar that is capable of acting as a reducing agent because it

has a free aldehyde group or a free ketone group.

 All monosacharides are reducing sugar along with some disaccharides,

oligosaccharides and polysaccharides.

Reagents: Fehling’s solution I and II, potassium fero-cyanide, zinc acetate, methyl blue

indicator, distilled water.

Apparatus: Retort stand, burette, conical flask, (heating mantle) not plate, volumetric

flask, funnel, filter paper, measuring cylinder.

Procedure:

1) Take 10ml of the sample in 200ml volumetric flask.

2) 5ml of zinc acetate and potassium fero-cyanide (10%) is added to volumetric flask,

shake to attain homogeneity and made up to 200ml mark with distilled water, close

and shake well.

3) The resulting solution is filtered using filter paper into another 200ml volumetric

flask.

4) Fill a 50ml burette with the titrate.

5) Measure each of Fehling’s solution I and II into a 250ml conical flask.

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6) Titrate the contents of the conical flask against the sugar solution in the burette by

running 15ml first and observing colour change while heating on a hot plate.

7) Add 3 drops of methyl blue indicator and continue titrating until the blue colour is

discharged and a brick red colour is obtained at the bottom which indicates endpoint.

Calculation:

(Initial dilution) x titre value equivalent /titre value x 1

100 x 100

b) Determination of total sugar

Total sugar is a measurement of sucrose and reducing sugars.

Any sucrose present in a sample must be broken down (inverted) into its individual

components parts, glucose and fructose, before running total sugar analysis.

Procedure:

i) Measure 50ml of the filtrate into a 100ml volumetric flask, add 5ml of conc. HCL.

ii) Shake and allow for 24hours (inversion of sucrose).

iii) Add few drops of phenolphthalein indicator.

iv) Neutralize the inverted sugar solutions with 50% NaOH until colour changes to pink.

v) Make up the solution with distilled water to the 100ml volumetric flask.

vi) Pour the prepared solution into the burette.

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vii) Pour 5ml each of Fehling’s solution I and II into a conical flask.

viii) Titrate the content of the conical flask against the sample in a burette by running

15ml of the sample while heating on a hot plate

ix) Add 3 drops of methyl blue indicator and continue to titrate until a brick red colour is

visible indicating end point.

Calculation:

TVE 1 1 100
Total sugar = initial dilution  x x x
TV 50 1000 1

Title: Determination of total volatile Nitrogen (TVN) in frozen fish

Total volatile Nitrogen is a parameter that measures the presence of volatile nitrogenated

basis in the raw material and fish meal.

Aim: To check for the level of spoilage in frozen fish.

Apparatus: Macro-kjehdal, ceramic mortar and pistol, 50ml beakers, 250ml conical flash,

distillation cylinder, weighing balance, spatula.

Regents: 2% Boric acid, 4% screen methyl red, 0.01NH2SO4 distilled water.

Procedure:

1) Cut/pound little quantity of the frozen fish sample with a ceromic mortar and pistol.

2) Weigh 2g of the sample into a beaker.

3) Transfer the sample into the distillation flask together with 250ml of distilled water

and pieces of anti-bomb.

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4) Fix the flask on the distillation stand of the kjehdal unit.

5) Rinse a conical flask with 2% boric acid.

6) Add 25ml of 2% boric acid and 2 drops of screen methyl red in a conical flask.

7) Fix the conical flask at the receiving end of the distillation stand.

7) On the water rap and the electric voltage faced on the kjehdal stand.

8) Allow it to distill until the conical flask reaches 100ml. Remove the conical flask and

allow it to cool.

9) Prepare your blank in the same procedure.

10) Titrate both your sample and your blank 0.1NH2SO4 to get a pink colour change

11) Record your titre value.

Calculation:

Total volatile nitrogen = (titre value of sample – titre value of blank) x 14

Limit – 30mg (max).

Title: Radiation test in stockfish and frozen fish

Aim: To detect and quantify the presence of radioactive elements in the fish.

Apparatus: Radiation meter.

Procedure:

1) The fish sample was brought out of the container and placed on flat surface.

2) After fixing and setting the radiation meter, the probing part of the radiation meter

was placed a little bit high above the fish sample.

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3) The reading then was calculated directly from the machine.

Note: Radiation is measured in Becquerel.

Title: Determination of salt (sodium chloride) in food samples.

Aim: To determine the amount of Nacl present in food sample.

Principle: The addition of standard AgNO3 to a sample solution using potassium

dichromate.

Apparatus: Burette conical flask, spatula, measuring cylinder, volumetric flask.

Reagents:
AgNO3 (silver Nitrate), K2CrO4 (potassium dichromate) indicator, distilled water.

Procedure:
1) A clean burette was filled with 0.1N AgNO3.

2) An already ashed samples was filtered with distilled water into a 100ml volumetric

flask.

3) 10ml of the filterate was poured into a conical flask, then 2 drops of potassium

dichromate indicator was added into it.

4) Then, the sample was titrated against 0.1N silver nitrate (AgNO3) and titre value

taken.

Calculation:

(dilution ) (100)
% salt content = (TV x vol of sample used) (salt factor)
10

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2.3 WATER CHEMISTRY LABORATORY

Water samples are analysis in this laboratory.

Analysis are divided into two; physical analysis and chemical analysis.

Physical analysis: Is the first analysis carried out.

It is done by physically examining the water, and it includes;

Appearance:

This is done to check to for suspend particles and also cloudiness in water sample.

Procedure:

The water sample was poured into a 1000ml beaker and swirled, position, the beaker was

observed to check for the presence of suspended and settled particles.

Net volume:

This is done to check if the measured volume complies with the manufacturers given

volume.

Procedure:

The water sample was poured into a clean measuring cylinder and the volume was

recorded. If the water is not up to the specify volume, an average of three measurements

was taken as the volume of the water sample.

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Odour:

This is done by perceiving the water as soon it is opened.

Chemical analysis

There are 2 methods used in chemical analysis:

(1) Bench method: It is the titration of water samples with specified indicators against

stipulated titrants in the fume hood (fume cupboard).

The analysis carried out include; chloride test, alkalinity test, CO2 test, and they

follow the same procedure but differ in the type of indicators and titrants used.

Apparatus:

Fume hood, conical flask, measuring cylinder, burette.

Procedure:

i) Set up the retort stand in the fume hood.

ii) Rinse and fill the burette with specified titrant.

iii) Measure 50ml of the water sample into a conical flask and add 3 drops of stipulated

indicator.

iv) Titrate against the titrate and take your reasoning

(a) Chloride test:

Titrant: 0.1N silver Nitrate (AgNO3)

Indicator: Potassium dichromate (K2CrO4)

Range: 0.00 - 200mg.

31
(b) Alkalinity test:

Apparatus: La motte Alkalinity test kit

Titrant: 0.02N H2SO4

Indicator: Methyl orange

Range: 0.00 – 100mg

(2) Automated method:

This involves the use of devices like the pH meter, conductivity meter, and the smart

spectrophotometer. This method make use of special kits with regards to the metal

compound of interest.

pH:

pH stands for ‘Potential hydrogen’ which is referred to the measure of degree of acidity or

alkalinity of water or food.

All water samples according to standard must be neutral and ranges from 6.5-8.5.

Aim: To determine neutrality of water sample.

Apparatus: Beaker, meter.

Procedure:

i) The pH meter is firstly caliberated with buffer 7 solution and must be either 6.99 +

0.01 or 7.00.

32
ii) Then pH meter rod (electrode) is being inserted fully into the beaker containing the

water sample.

iii) The enter button on the pH meter is pressed, the meter starts reading until the

reading stops.

iv) Then take your value, and rinse the electrode with distilled water before hanging.

Range 6.5-8.5

(b) Conductivity and total solid determination:

 Conductivity refers to the ability of a material (water) to conduct or allow the flow

of electric currents or heat. Ranges from 0.00-19.0

 Total solid is the amount of minerals and salt impurities in water samples.

Aim: To determine the conductivity and total solid in water samples.

Apparatus: Beaker conductivity meter.

Procedure:

i) Calibrate the conductivity meter rod (electrode) with 1.01 NKCL (potassium

chloride) rinse with water before inserting into the water sample.

ii) Insert the rod into the beaker containing the water sample and press the enter button.

iii) Take the reading as your conductivity value (M/S), then press the TS button to get

your total solid value (mg/l).

iv) Rinse the electrode with distilled water before hanging back.

33
 Range 0.00-19-0.

TDS range – drinking water (500ppm)

Water for agriculture (1200ppm)

Suspended solid = total solid – total dissolved solid

c) Calcium and Magnesium (Hardness)

Reagent: Ca and Mg indicator

Procedure:

i) Scan blank with the sample in the cuvette.

ii) Add your sample into the cuvette containing Ca and Mg indictor.

iii) Scan and take your reading

Calculation:

Magnesium = 1 x value
3

Calcium = 2 x value
3

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2.4 MICROBIOLOGY LABORATORY

Microbiology laboratory is where food and water samples are analyzed and diagnosis to

identify the microbial load

Microbiology laboratory is made up of four different rooms, preparation, room, water

laboratory, food laboratory and incubation.

The analysis carried out are aimed at identification of micro-organism present in a sample.

It is basically a quantitative analysis laboratory.

Types of analysis carried out in the laboratory:

Enumeration of Aexbic mesophilic count, mould count, Escherichia, coli, salmonella and

shigella count, pseudomonas, coliform bacateria.

Types of media

In microbiology ‘culture media’ is any liquid solid or sediment preparation made

specifically for the growth, storage, or transport of micro-organisms. Microorganisms

analyzed in the lab include, mould bacteria, algae fungi etc.

The variety of media that exist for the culturing of specific micro-organisms such as;

general media, differential media, selective media, enriched media.

1) General media: This type of media supports the growth of different types of micro-

organisms. E.g Nutrient agar, plate count agar, thioglycollate broth etc.

35
2) Differential media: This type of media allows the growth of some micro-organisms

and differentiates them according to colours e.g violet red bile, agar, chromocult

agar etc.

3) Selective media: This type of media allows the growth of a particular micro-

organism e.g centrimide agar etc.

4) Enriched media: This type of media needs to be enriched to allow the growth of

micro-organism. E.g centrimide agar enriched with glycerol, buffered peptone water

etc.

Preparation of Media:

Media are prepared in the media preparation room. To prepare media, the volume of

sample to be prepared needs to be considered which is based on the number of samples

needed to be inoculated. The formula for the amount of media to be prepared is; (Required

volume x mass volume)/1000.

N/B: The mass volume is written on the body of the media container.

Procedure for media preparation:

i) The amount of media to be prepared in measured first through the formula and

weighed.

ii) The media is poured into the media bottles with the addition of the required volume

of water.

36
iii) The media was then autodialled at 1210C at 15 Psi (pounder per square inch) for 15

minutes for sterilization, cooled and transferred into the water bath to maintain the

temperature at 450C.

iv) The media is transferred into the petri-dishes for inoculation.

N/B: Some media are heated and not autoclaved.

 Example of some media and their functions:

a) Centrimide Agar (CA): It is used for detection of pseudomonas in water.

b) Violet red bile Agar (VRB): It is used for the detection of E.coli (a spindle shape

colony indicates the presence of E. coli).

N/B: This media is not autoclave put heated in a heating mantle with frequent swirling

until it boils.

c) Plate count Agar (PCA): It is used for detection of aerobic mesospheric bacteria.

d) Salmonella shigella Agar (SSA): It is used for detection of salmonella.

e) Buffered peptone water: It is used for the detection of salmonellae.

f) Lauryl sulfate broth (LSB): It is used for the detection of coliform.

g) XLD Agar (xylose-lysin-descoxycholat agar): It is an enrichment media, used for

the detection of salmonella.

37
The two controls during inoculation include;

Closed control: This is done to know if the media was properly media it if there is growth

it means the media was not well prepared, it is done by pouring the media into a petri-dish

and close it.

Open control: This is done to know the microbial load of the environment where the

analysis is been carried out. It is done by pouring the media in a petri dish and leaving it

open for some time. If there is growth it means the environment was not well sterilized.

Inoculation of samples

i) The work bench was swapped with ethanol and cotton wool.

ii) Laboratory numbers assigned to samples and petri-dishes labeled according to media

for easy identification.

iv) The prepared media was poured 15-20ml into the petri-dish after dispensing

1ml of the sample into it; strictly for PCA and VRB (because the E. coli and

aerobic mesophiles checked for are facultative anaerobes and can grow above

or beneath the media; also VRB is poured twice after the first has solidify

because E. coli easts up the media). But, for CA, the media is poured first and

allowed to solidify before adding 1ml of the sample. (Because pseudomonas

are obligate aerobes and needs only oxygen to grow and so should be on top of

the media.

38
 iv) In the case of coliform, the dougham tube is dropped downwards or inverted into the

bijou bottles, then 1ml of the sample was pipetted into the lauryl sulphate broth

(LSB). The dougham tube in the bijou bottle was filled with the broth by swirling the

bottle.

v) Incubate the inoculated plates at 370C for 48 hours. Then observation were made to

know if there were growths while in the case of LSB growth (coliform) is detected

when the media which fills the dougham tube is decreased.

Numeration Of Micro-Organisms And Media Used

S/N Microbial Description of microbe Sources Media used Observation

type

1 Aerobic Grows at room Food and Plate count agar Pinkish red or

mesophili temperature in the water PCA yellow

bacteria presence of oxygen

2 Escherichia Gram negative facultative Food and Chromocult Pinkish spindle

coli anaerobic rod. water feacally Agar (CRA shaped colonies

- In intestine of warm contaminated TBX) in between the

blooded animals. violet red bile two agar layers

- Some cause of food agar VRB

poisoning

3 Pseudomonas Gram negative rod with Water Centrimide agar Greenish-lemon

popular flagella- some (CA) enriched coloration

39
 produce spores and are with glycerol

harmful general

4 Mould Gram positive Food Potato dextrode Discolouration

agar (PDA) of food and off

odour – produce

myacotoxins e.g

Aflatoxin

5 Coliforms Gram negative facultative Food and - lauryl sulphate ferments lactic

anaerobic rod water broth (LSB) acid to give out

- Chromocult gas.

coliform agar

(CRD)

6 Salmonella Gram negative anaerobic Food Salmonella and - Yellow spot

and shigella rods (yoghurt) shigella agar with black

(SSA) center.

40
 CHAPTER THREE

3.1 NEW SKILL ACQUIRED

1) The SIWES experience has really helped me to break the barrier between theoretical

knowledge and its practical by being able to apply the analytical principles of the

classroom to the real practical work in the agency.

2) It gave me access to understand better the relevance of my course of study to the

development of my society.

3) The schemes provides me the opportunity to understand the way NAFDAC safe

guard the health of our nation.

3.2 PROBLEMS ENCOUNTERED

During the SIWES programme, the problems in encountered include;

1) Lack of finance as a result of no payment.

2) Inability to be allowed to operate some biochemical equipments due to fear of their

break down as a result of their high purchasing cost. E.g PHLC (high Pressure Light

Cromatography, AAS (Atomic absorbance spectrophotometer).

41
3.3 CONCLUSION

In conclusion, I would say that the objectives of student industrial work Experience

scheme (SIWES) has been achieved by exposing me to the environment of work and also

making the transition from school environment to work environment easier.

3.4 RECOMMENDATION

 There should not be limitation to machines or equipments that are been used in the

industrial field.

 I recommend that the university should take practical work more seriously; this

will help students to fit in well during industrial training.

 I also recommend that the government should mandate or instruct all industries

and Agencies to give out allowances no matter how small to students serving in

their establishment.

42
 REFERENCE

Nafdac (1994) Standard Operating Procedures, Food Laboratory.

Nafdac (1994) Standard Operating Procedures, Water laboratory.

Ayo, J. A. K., and Agu, H. O. (2014) Simplified Manual of Food Analysis for Tertiary and

Research Institutions, Vol. 1.

RSU (2016) SIWES Handbook

43
Inoculation of water samples Crosschecking of bijou bottles containing LSB
(Lauryl Sulphate Broth) and water samples

Autoclave Muffle Furnace

44
 Kjehdal Stand

Smart spectrophotometer

Water bath PH meter

45
46