Siwes Report - 2021

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A TECHNICAL REPORT

ON

STUDENT INDUSTRIAL WORK EXPERIENCE SCHEMES (SIWES)

AT

EMACHY CHEMICAL AND LABORATORY SERVICES,

NO. 183, EGBEDA-IDIMU ROAD, ABULE-ODU BUS-STOP,

EGBEDA LAGOS STATE

BY

IHUOMA OKECHUKWU SOLOMON

MATRIC NO: 160403044

SUBMITTED TO THE

DEPARTMENT OF CHEMICAL SCIENCES

FACULTY OF SCIENCES

OLUSEGUN AGAGU UNIVERSITY OF SCIENCE AND

TECHNOLOGY

OKITIPUPA, ONDO STATE

IN PARTIAL FULFILLMENT FOR THE AWARD OF BACHELOR OF


TECHNOLOGY (B.TECH) IN INDUSTRIAL CHEMISTRY

AUGUST, 2021
DECLARATION

I, Ihuoma, Okechukwu Solomon hereby declare that this report was written by me. All

sources of information are clearly acknowledged by means of references.


CERTIFICATION

This is to certify that this industrial training was carried out by Ihuoma Okechukwu

Solomon with matric number; 160403044 of the chemical department Olusegun Agagu

University of Science And Technology, Okitipupa, Ondo State, at EMACHY CHEMICALS

AND LABORATORY SERVICES.

_____________________ _____________________
Dr. (Mrs.) E. T. Omotade Date
(SIWES Supervisor)

_____________________ _____________________
Dr. O. P. Osarumwensen Date
(SIWES Coordinator)

_____________________ _____________________
Dr. O. A. Oladimeji Date
(Ag. H.O.D Chemical Sciences)
DEDICATION

This project is dedicated to the Ancient of days Almighty God who in His mercies and

unsearchable wisdom grant me the ability and capacity to successfully complete my

industrial training and to my parents for their support.

iv
ACKNOWLEDGEMENT

Doxology to Almighty God for his love over my life his mercies and goodness has always

been there for me all glory and honor belongs to you Lord.

To Mr. IHUOMA OLIVER and Mrs. IHUOMA CHINERE. I am very grateful for your care,

love and support. My special thanks also go to Mrs. KELECHUKWU for the care, love and

support, it will always be remembered. I will also love to appreciate my siblings, cousins,

uncle, and especially my aunt in person of Miss IHUOMA FAUSTINA.

I won’t forget to thank those that made EMACHY CHEMICAL AND LABORATORY an

interesting place for me; the laboratory analysts in person of MR OLABODE ADEDIYA

who was always willing to impact knowledge and also my colleague (students and analyst)

whom we learned together. My story won’t be complete if I hadn’t met you guys.

Finally, my acknowledgement will be incomplete if I fail to appreciate the Head of

Department, level Advisor, both teaching and non- teaching staff of the Chemical Department

.a big thank you to my friends and family. Thank you all, may the Almighty God bless you

v
Table of Content

DECLARATION..............................................................................................................................ii

CERTIFICATION...........................................................................................................................iii

DEDICATION..................................................................................................................................iv

ACKNOWLEDGEMENT................................................................................................................v

Table of Content...............................................................................................................................vi

List of Table.....................................................................................................................................vii

List of Plate.....................................................................................................................................viii

ABSTRACT......................................................................................................................................ix

CHAPTER ONE...............................................................................................................................1

1.1 INTRODUCTION ABOUT SIWES.........................................................................................1

1.2 BRIEF HISTORY OF SIWES..................................................................................................1

1.3 AIMS AND OBJECTIVES OF SIWES...................................................................................2

1.3.1 AIM....................................................................................................................................2

1.3.2 OBJECTIVES....................................................................................................................2

CHAPTER TWO..............................................................................................................................4

2.1 HISTORY OF EMACHY CHEMICALS ANDLABORATORY SERVICES........................4

2.2 OUR VISION............................................................................................................................4

2.3 OUR MISSION.........................................................................................................................5

2.4 OUR QUALITY POLICY........................................................................................................5

THE ORGANOGRAM OF THE COMPANY...............................................................................6


Organizational Chart ......................................................................................................................6

Plate 2.1: Emachy Staff and IPAN Team.......................................................................................7

CHAPTER THREE..........................................................................................................................8

3.0 LABORATORY.......................................................................................................................8

3.1 LABORATORY MAINTENANCE.........................................................................................8

3.1.1 Cleaning.............................................................................................................................9

3.1.2 Calibration..........................................................................................................................9

3.1.3 Repairs.............................................................................................................................10

3.1.4 Refurbishing.....................................................................................................................10

3.2 LABORATORY PRECAUTION...........................................................................................10

3.2.1 Follow the instruction..........................................................................................................10

3.2.2 Know the Location of Safety Equipment.............................................................................11

3.2.3 Put on Protective Ware....................................................................................................11

3.2.4 Don't eat or Drink in the Laboratory................................................................................11

3.2.5 Don't Taste or Sniff Chemicals........................................................................................11

3.2.6 Dispose of Lab Waste Properly.......................................................................................12

3.2.7 Know What to Do with Lab Accidents............................................................................12

3.2.8 Leave Experiments at the Lab..........................................................................................12

3.3 ANALYTICAL CHEMISTRY LABORATORY..................................................................13

Table 3.1: LABORATORY EQUIPMENT AND FUNCTION...................................................14

CHAPTER FOUR...........................................................................................................................18

4.0 PHYSICO-CHEMICAL ANALYSIS.....................................................................................18


4.1 PHYSICO-CHEMICAL ANALYSIS OF WATER...............................................................18

4.1.1 TEST FOR ALKALINITY IN WATER (CRISP METHOD).........................................18

4.1.2 DETERMINATION OF CHLORIDE IN WATER (ARGENTIOMETRIC METHOD)20

4.1.3 DETERMINATION OF TOTAL HARDNESS OF WATER.........................................21

4.1.4 DETERMINATION OF IRON IN WATER (Phenanthroline).......................................22

4.1.5 DETERMINATION OF PH............................................................................................23

4.1.6 DETERMINATIONOF TOTAL DISSOLVED SOLID.................................................23

4.2 PHYSICO-CHEMICAL ANALYSIS OF FOOD...................................................................24

4.2.1 DETERMINATION OF FAT CONTENT......................................................................24

4.2.2 DETERMINATION OF CRUDE PROTEIN..................................................................25

4.2.3 DETERMINATION OF MOISTURE CONTENT.........................................................27

4.2.4 DETERMINATION OF SPECIFIC GRAVITY.............................................................28

4.2.5 DETERMINATION OF TITRATABLE ACIDITY.......................................................29

4.2.6 DETERMINATION OF ASH CONTENT......................................................................29

4.2.6 DETERMINATION OF ENERGY.................................................................................30

CHAPTER FIVE.............................................................................................................................32

5.0 SUMMARY OF ATTACHMENT ACTIVITIES..................................................................32

5.1 PROBLEMS ENCOUNTERED DURING THE PROGRAM...............................................32

5.2 SUGGESTION FOR IMPROVEMENT OF THIS SCHEME...............................................32


List of Table

Table 3.1: LABORATORY EQUIPMENT AND FUNCTION.......................................................16


List of Plate

Plate 2.1: Emachy Staff and IPAN Team...........................................................................................8


ABSTRACT

This is a comprehensive report on my SIWES program at the Emachy Chemical and laboratory

service (ECLS). ECLS is an analytical laboratory that specialize in testing of water, foods,

chemicals, cosmetics, medical devices, effluents and Herbal products. The report covers the work

done during my stay with the company and the experience gained from the laboratory unit. The

major work presented in this report includes: standard ISO and IPAN practices in water and food

testing of pH, Alkalinity, Electrical Conductivity, Total Dissolved Solid (TDS), Total Suspended

Solid (TSS), Free CO2, total Iron contents, total hardness, total chloride content, for food moisture

content, Fat, Protein, Acidity, moisture content, specific gravity, titratable acidity, ash content,

energy
CHAPTER ONE

1.1 INTRODUCTION ABOUT SIWES

The Students’ Industrial Work Experience Scheme (SIWES) is a skill training program

designed to expose and prepare students of universities, polytechnics and Colleges of

Education for the industrial work situation they are likely to meet after graduation. The

scheme also affords students the opportunity of familiarizing and exposing themselves to the

needed experience in handling equipment and machinery that are usually not available in their

institutions.

1.2 BRIEF HISTORY OF SIWES

Before establishment of the scheme, there was a growing concern among our industrialists

that graduates of institutions of higher learning lacked adequate practical background studies

preparatory for employment industries. Thus the employers were of the opinion that the

theoretical education going on in higher institutions was not responsive to the needs of the

employers of labor. It is against this background that the rationale for initiating and designing

the scheme by the fund during its 1 formative year – 1973/74 was introduced to acquaint

students with the skills of handling employers’ equipment and machinery. The ITF solely

funded the scheme during its formative years. But as the financial involvement became

unbearable to the fund, it withdrew from the scheme in 1978. The federal government handed

over the scheme in 1979 to both the National Universities Commission (NUC) and the

National Board for Technical Education (NBTE). Later, the federal government in November

1984 revert the management and implementation of the scheme to ITF and it was effectively

taken over by the Industrial Training Fund (ITF) in July 1985 with the funding being solely

borne by the federal government.


1.3 AIMS AND OBJECTIVES OF SIWES

SIWES is strategized for skill acquisition. It is in fact designed to prepare and expose students

of universities, polytechnics and colleges of education to the real-life work situation they

would encounter after graduation.

Therefore, SIWES is key factor required to inject and engender industrialization and economic

development in our nation through the induction of scientific and technological skills on

students.

1.3.1 AIM

The aim of SIWES is to bridge the gap between theory and practical work in order

tosharpenstudents’skillsandunderstandingofphysicalplanningandpracticesonthevariousfields.

1.3.2 OBJECTIVES

The main objective of SIWES includes the following:

i. To provide an avenue for students in industries to acquire industrial skills and

experience in their various field of study.

ii. To provide students the chance to apply their knowledge in real work situation

thereby bridging the gap between theory and practical’s.

iii. To make the process of exchange from school to world of work and enhance

students contact for later job placement.

iv. To expose students to work, methods and techniques in handling equipment’s and

machines that may not be available in their institutions.

v. To make the transition of students from university to industries upon graduation

easy.
vi. To enlist and strengthen industry’s involvement in university education.

vii. To satisfy accreditation requirement set by National University commission.

viii. To enable university educators access the effectiveness of their curriculum and make

modification where necessary.


CHAPTER TWO

2.1 HISTORY OF EMACHY CHEMICALS ANDLABORATORY SERVICES

Emachy Chemicals and Laboratory Services is a laboratory facility registered in the year 2009 to

provide quality laboratory testing services in the areas of water, food, cosmetics, and raw

materials. We have our head office and laboratory facility at No. 183 Egbeda- Idimu Road, Abule-

Odu Bus stop, Egbeda, Lagos. We also have an Annex Office at No 18 Abbi Street, Mende,

Maryland, Lagos. We are corporate member of the Institute of Public Analysts of Nigeria

(IPAN).The Institute of Public Analysts of Nigeria was established by decree No. 100 of 1992,

now ACT CAP116 LFN 2004 to, among other functions, regulate Laboratory practice and

management in Nigeria. The laboratory (Emachy Chemicals and Laboratory Services) provides

analytical testing and consultation services in the areas of food, water, chemicals, and related

industrial raw materials. EMACHY CHEMICALS AND LABORATORY SERVICES is an

analytical laboratory that Specialize in testing of water, foods, chemicals, cosmetics, medical

devices, effluents and Herbal products. We are known in the field of products analysis and testing,

water treatment and have been innovating our We have the right team, the right experience, the

right tools, and the right approach to render these professional services at effective cost, best

quality and time. Your satisfaction is our happiness and pride.

We maintain: Fast, efficient turnaround of result complete clients confidentiality Independent

testing and advice fast and flexible response to your needs.

2.2 OUR VISION

To be the analytical laboratory of choice by partnering with our clients to deliver quality analytical

services in support of their business plan for growth, product quality and brand preservation.
2.3 OUR MISSION

To integrate analytical solutions and quality systems that generate the highest confidence in

the data reported to our clients. To provide consistent, reliable and affordable independent

services to our customers by means of approved methodology, state of the art technology

efficient customer service and knowledgeable technical support.

2.4 OUR QUALITY POLICY

We are committed to the use of very qualified man power, appropriate equipment and

methods that deliver quality laboratory tests and test results/reports that consistently meet the

requirements of our clients within the provision of relevant laws and regulations and in

accordance with the requirements of the International Standard (ISO 17025:2017)

Services constantly in keeping updated with the changes taking place in the industry.
THE ORGANOGRAM OF THE COMPANY
Organizational Chart

LAB DIRECTOR/ QUALITY


MANAGER

EXTERNAL AUDITOR INTERNAL AUDITOR TECHNICAL MANAGER

ANALYST 1

ANALYST 2

ANALYST 3
Plate 2.1: Emachy Staff and IPAN Team
CHAPTER THREE

3.0 LABORATORY

A laboratory is a facility that provides controlled conditions in which scientific or

technological research, experiment and measurement may be performed. A laboratory can

also be defined as a building equipped for experimental study in a science or for testing and

analysis. Laboratories used for scientific research take many forms because of the differing

requirements of specialists in the various fields of science and engineering. A physics

laboratory might contain a particle accelerator or vacuum chamber, while a metallurgy

laboratory could have apparatus for casting or refining metals or for testing their strength. A

chemist or biologist might use a wet laboratory, while a psychologist's laboratory might be a

room with one-way mirrors and hidden cameras in which to observe behavior. In some

laboratories, such as those commonly used by computer scientists, computers (sometimes

supercomputers) are used for either simulations or the analysis of data. Scientists in other

fields will use still other types of laboratories. Engineers use laboratories as well to design,

build, and test technological devices. Types of laboratory includes: analytical chemical

laboratory, clinical and medical laboratories, production laboratories, research and

development laboratories etc.

3.1 LABORATORY MAINTENANCE

Without a spotless lab in which to work, the risk of cross-contamination is likely making good

housekeeping almost as important to your work as the study itself. And, the benefits of good

lab maintenance don’t end there. Equipment is often one of the biggest outlays in a lab so

taking adequate care of what you have


3.1.1 Cleaning

1. Carry out a daily wipe down of all equipment exteriors

2. Lab cleanliness is one of the easiest, most affordable and most obvious ways to keep your

lab in great shape but surprisingly is often overlooked

3. Carry out a weekly deep clean of all equipment

4. Carry out a regular deep clean of microscopes using a 70:30 mixture of ether and alcohol –

this ensures that they are sufficiently clean to yield most accurate results

5. Consult the manual or lab manager on any specific processes for cleaning demanding

equipment

6. Consider outsourcing cleaning of challenging items to a qualified professional

7. Following these simple cleaning procedures will keep equipment in peak condition so that

your lab runs without a hitch

3.1.2 Calibration

Failure to regularly calibrate equipment can lead to a lack of accuracy with your data which

could end up disrupting entire experiments. There are various services available to ensure

your equipment is regularly calibrated and done so to the right standard.

It’s advisable to:

Carry out an inventory of your equipment and decide which is most suitable for each item – from

basic preventative maintenance to more advanced accuracy verification.

Regularly calibrate equipment for ongoing preventative maintenance that will keep your lab sharp.
3.1.3 Repairs

From time to time, lab items will wear out and stop working. But, rather than immediately

disposing of faulty equipment, take the time to see if parts could be replaced or items can be

repaired instead.

It’s likely that equipment can be updated and maintained rather than simply disposed of.

Particularly with larger items, repairing and replacing parts can be an effective way to increase

lifespan and keep down costs. Due to the nature of the items, some parts will wear quicker

than others but, when adequately managed, these can be replaced in time to prevent problems

or burnout. Consider centrifuges, filtration systems and microscope lenses, each of these can

be simply replaced without the need to dispose of the entire machine.

3.1.4 Refurbishing

Refurbishing refers to the process of dismantling pieces of laboratory equipment and cleaning

each component part thoroughly. Metal elements are also polished and any pipette pistons can

be lubricated. Refurbishing at regular intervals will extend the life of your laboratory

equipment and increase its efficiency and functionality.

3.2 LABORATORY PRECAUTION

3.2.1 Follow the instruction: Listen to your instructor or lab supervisor and follow procedure

stated in the standard operating procedure journal, it's critical to listen, pay attention, and be

familiar with all the steps, from start to finish, before starting the experiment. If unclear about

any point or have questions, get them answered before starting, even if it's a question about a

step later on in the protocol. Know how to use all of the lab equipment before start
3.2.2 Know the Location of Safety Equipment: In the experiment something goes wrong,

it's important to know the location of the safety equipment and how to use it. It's a good idea

to periodically check equipment to make sure it is in working order. For example, does water

actually come out of the safety shower? Does the water in the eye wash look clean.

3.2.3 Put on Protective Ware: Dress for the lab. This is a safety rule because your clothing is

one of your best forms of protection against an accident. For any science lab, wear covered

shoes, long pants, and keep your hair up so it can't fall into your experiment or a flame. Make

sure you wear protective gear, as needed. Basics include a lab coat and safety goggles. You

may also need gloves, hearing protection, and other items, depending on the nature of the

experiment.

3.2.4 Don't eat or Drink in the Laboratory: Save your snacking for the office, not the lab.

Don't eat or drink in the science laboratory. Don't store your food or beverages in the same

refrigerator that contains experiments, chemicals, or cultures. There is too much risk of

contaminating your food. You could touch it with a hand that is coated with chemicals or

pathogens or set it down on a lab bench that has residue from past experiments. Having drinks

in the lab risks your experiment, too. You could spill a drink on your research or lab notebook.

Eating and drinking in the lab is a form of distraction. If you are eating, you aren't

concentrating on your work. If you're used to drinking liquids in the lab, you might

accidentally reach for and drink the wrong liquid. This is especially true if you did not label

your glassware or used lab glassware as dishes.

3.2.5 Don't Taste or Sniff Chemicals: Tasting or smelling some chemicals can be dangerous

or even deadly. The best way to know what's in a container is to label it, so get in the habit of

making a label for glassware before adding the chemical.


3.2.6 Dispose of Lab Waste Properly: Most labs have dedicated waste containers for sharps,

bio-hazardous waste, radioactive waste, and organic chemicals. One important laboratory

safely rule is to know what to do with your experiment when it's over. Before you start an

experiment, you should know what to do at the end. Don't leave your mess for the next person

to clean up. Are the chemicals safe to dump down the drain? If not, what do you do with them

If you have biological cultures, is it safe to clean up with soap and water or do you need an

autoclave to kill dangerous organisms? Do you have broken glass or needles? Know the

protocol for disposing of "sharps".

3.2.7 Know What to Do with Lab Accidents: Accidents happen in the lab, so know how to

respond before they occur. Accidents happen, but you can do your best to prevent them and

have a plan to follow when they occur. Most laboratories have a plan to follow in the event of

an accident. One particularly important safety rule is to tell a supervisor if and when an

accident occurs. Don’t lie about it or try to cover it up. If you get cut, exposed to a chemical,

bitten by a lab animal, or spill something there could be consequences, and the danger isn’t

necessarily only to you. If you don’t get care, sometimes you could expose others to a toxin or

pathogen. Also, if you don’t admit to an accident, you could get your lab in a lot of trouble.

3.2.8 Leave Experiments at the Lab: Don't take chemicals or lab animals home with you.

You put them and yourself at risk. It's important, for your safety and the safety of others, to

leave your experiment at the lab. Don't take it home with you. You could have a spill or lose a

specimen or have an accident. This is how science fiction movies start. In real life, you can

hurt someone, cause a fire, or lose your lab privilege while you should leave lab experiments

at the lab, if you want to do science at home, there are many safe science experiments you can

try.
3.3 ANALYTICAL CHEMISTRY LABORATORY

Analytical chemistry laboratory is laboratory that studies and uses instruments and methods

used to separate, identify and quantify chemical sample. In practice, separation, identification

or quantification may constitute the entire analysis or be combined with another method.

Separation isolates analytes. Qualitative analysis identifies analytes, while quantitative

analysis determines the numerical amount or concentration.


Table 3.1: LABORATORY EQUIPMENT AND FUNCTION

NAME PICTURE USES


RING STAND Supports the Bunsen burner, iron
ring, pipe stem triangle, and other
items, often while heating a
substance.

BEAKER Holding water (also used to heat


liquids

VOLUMETRIC Flask calibrated to contain a precise


volume at a particular temperature.
FLASK
Used for precise dilutions and
creating standard solutions.

MORTAL AND Used to grind chemicals to powder


PESTLE
WIRE GAUZE Suspending glassware over
the
Bunsen burner
TONG Transport a hot beaker; remove lid
from crucible.

WIRE BRUSH Used to clean the inside of test tubes


or graduated Cylinders

FUNNEL Used to pour liquids into containers


with small openings; also used to
hold filter paper

GRADUATED Measuring specific


amounts of liquids
CYLINDER
SPATULA Measuring/removing small amounts
of solids or powders (often when
obtaining mass)

WASH BOTTLE Used to wash down specific pieces


of equipment with water or keep
materials moist.

BURETTE Measuring specific


amounts of liquids
(often
determining amounts of acids or
bases needed
) releasing small amounts of acids or
bases into other solutions

DROPPER Used to obtain small amounts of


liquids (not precise)

THERMOMETER Used to measure temperature

PIPETTE Used to measure and dispense small


amounts of liquids

SEPARATING
FUNNEL
HOT PLATE Used for consistent heat; used to heat
substances that may be flammable.
ANALYTICAL This is used for measuring the
masses of objects such as Petri dish,
WEIGHING
filter papers etc. in the laboratory.
BALANCE

A pH (potential of Hydrogen)
measurement reveals whether a
PH METER
solution is acidic, alkaline (basic) or
neutral. Very soft water is usually
acidic while very hard water is
usually alkaline (with exceptions).
The pH meter provides the means for
determining the acidity or alkalinity
of water.

CONDUCTIVITY Electrical conductivity refers to the


ability of a solution to conduct an
METER
electric current.
How does the conductivity meter
work?
Two electrodes with an applied AC
voltage are placed in the solution.
This creates a current dependent
upon the conductive nature of the
solution. The meter reads this current
and displays it in EC
HOT AIR OVEN A complete cycle involves heating
the oven to the required temperature,
maintaining that temperature for the
proper time interval for that
temperature, turning the machine off
and cooling the articles in the closed
oven till they reach room
temperature.

REFRACTOMETER This is used to measure degree brix


of beverage but unlike DMA, air
bubble does not affect the result as
its mode of operation is by
measuring the refractive index which
is converted to degree brix. It is
majorly used to measure the degree
brix of non- carbonated beverages
i.e. juices.
CHAPTER FOUR

4.0 PHYSICO-CHEMICAL ANALYSIS

This branch of analysis deal with inter relation between the composition and properties of

matter, it investigate the interrelation between the composition structure and properties as well

as determination of analytical component of samples to be analyzed. Physicochemical analysis

can be carried out on a wide variation of samples; sample includes food, water, drug,

cosmetics, metals etc.

4.1 PHYSICO-CHEMICAL ANALYSIS OF WATER

It is a way to meet the necessary standards of quality control and sanitary control; so several tests

are performed on water for quality control purpose.

4.1.1 TEST FOR ALKALINITY IN WATER (CRISP METHOD)

Alkalinity roughly refers to the amount of base in a solution that can be converted to

uncharged species of strong acids, but in terms of water alkalinity, alkalinity refers to the

capability of water to neutralize acids or the ability of water soaks proton without change in

pH. The word alkalinity came from an Arabic word AL-QULI it’s the ability of water to resist

change that would make it more acidic, and alkalinity in natural water is the presence of

bicarbonate, carbonate and hydroxide. It is determined by titrating the solution with a

monoprotic acid such as HCl, until the pH changes abruptly or reaches it endpoints.

Alkalinity is expressed in units Meq/l that is; (mgcaco3/l)

Meq/l= milli equivalent per litre, which corresponds to the amount of monoprotic acid added

as a titrant in millimeter per liter. It test the temporary hardness of water, and for raw water

ability to neutralize acidic pollution.


REASON FOR TEST

This test is carried out because some ion concentration does not change with change in PH,

the concentrations of such ion cannot be determined by change in PH, such ion are known as

consecutive ions. Examples include Na, Ca and Mg.

PRINCIPLE: Alkalinity is determined by adding a strong acid to the water sample until all

the ions listed above are converted to uncharged species, which is indicated by a change in

colour by the indicator added. It is not affected by temperature and pressure.

REAGENTS: Methyl Orange, Phenolphthalein, 0.1M Hydrochloric acid.

APPARATUS: 250ml conical flasks, 25ml pipette, 50ml burette, pipette-filler, retort stand, funnel

and beaker

PROCEDURE:

• Measure 25ml of water sample using a pipette into a dry clean conical flask.

• Add two drops of methyl orange indicator and stir.

• Add two drops phenolphthalein and stir.

• Pour acid into the burette and take initial readings.

• Titrate acid solutions in the burette against the solution in the conical flask until color

changes from orange to pink end point.

• Take final readings.

• Calculate total alkalinity:

Where N= Normality of Acid F=Acid Factor


4.1.2 DETERMINATION OF CHLORIDE IN WATER (ARGENTIOMETRIC METHOD)

PRINCIPLE: The maximum allowable chlorine concentration is 250mg/l in drinking water

and is established for reasons of taste rather than safeguard against physical hazard, due to the

fact that if sodium is present in water with chlorine of above 250mg/l chlorine possess a salty

taste.

The taste detection level may be a large amount in taste if chloride is present as calcium or

magnesium salt, and the large use of zeolite as water softener contributes to the presence of

water in waste waters potassium chromate can be used as an indicator in neutral or slightly

alkaline solution and employs titration with AgNO3. Standard solution which selective

precipitate with the chloride first then the chromate, the end point the titration is the first

appearance of the silver chromate precipitates.

APPARATUS: Conical flask, measuring cylinder, burette, pipette, retort stand.

REAGENTS: Potassium chromate (K2CrO4), 0.1M Silver nitrate (AgNO3)

PROCEDURE

 Transfer 25ml of sample into a 250ml conical flask

 Add one 1ml of potassium chromate indicator

 Titrate with standardized 0.1M AgNO3 to a brick-red end point

CALCULATION

Total Chlorine= Average Titre x 0.1M AgNO3 x 35400

Volume of sample
4.1.3 DETERMINATION OF TOTAL HARDNESS OF WATER

Hardness is defined as the characteristic of water which represents the total concentration of

calcium and magnesium expressed as their calcium carbonate equivalent when other

polyvalent metal ion are present. Insignificant amount they are also determined and report as

hardness.

REASON FOR ANALYSIS

Large amount of hardness are undesirable for aesthetics and economic research in many

industries and must be removed before the water can be used. Level above 500mg/l Hardness

are undesirable for domestic uses and above 250mg/l for drinking use

PRINCIPLE: The method assumes the presence of both calcium and magnesium which are

nearly always present in natural water. Some metal ions interfere with the procedure by

causing fading or indistinct end point, and this reduced by the addition of inhibitors KCN,

potassium cyanide.

APPARATUS: Conical Flask. Burette, Pipette, Retort Stand, Funnel.

REAGENT: Ammonia (NH3), Ethylenediamine-Tetraacetic Acid (EDTA), Erichrome Black-T

PROCEDURE

 Pipette 25ml of sample into a conical flask

 Add 1ml of ammonia buffer solution

 Add a pinch of Eriochrome black T to the solution

 Fill the burette with standard EDTA solution

 Titrate EDTA against solution in conical flask till color change to blue end point.
4.1.4 DETERMINATION OF IRON IN WATER (Phenanthroline)

This is to provide standard procedure for calculating the iron of water sample following standard

procedure

PRINCIPLE

The ferric form of iron is reduced to ferrous form by boiling with HCL and hydroxylamine

hydroxide, phenanthroline is then added to form soluble chelated complex of orange red color

with iron, the change in color obeys beers law.

EQUIPPMENT AND APPARATUS

DR/2000 Spectrophotometer at 510nm, cuvette, volumetric flask, measuring cylinder, conical

flask, and beakers

REAGENTS: Hydrochloric acid (HCl), Hydroxylamine hydrochloride, 1,10-Phenanthroline

monohydrate, Ammonium acetate.

PROCEDURE

 Take 50ml of sample into 125ml conical flask

 Add 2ml of HCL and 1ml of hydroxylamine solution to the solution in he conical flask

 Boil solution still volume reduce to about 15ml to 20ml

 Cool and transfer to a 50ml volumetric flask

 Add 10ml of ammonium acetate and 4ml of phenanthroline into the solution in the

volumetric flask

 Dilute solution to mark with distilled water

 Mix and allow for 10min-15mins for colour development


 Run blank on the spectrophotometer at stored program for ferrous iron using distilled water

as blank to zero the spectrophotometer

 Run readings of sample after colour has been developed on the spectrophotometer and take

readings

PRECAUTION

If the volume is expected to contain more than 2000mg iron uses a smaller portion and dilute to

50ml.

4.1.5 DETERMINATION OF PH

EQUIPMENT: pH meter

APPARATUS: Beaker

STANDARDS: Buffer 4,7,10 solutions

PROCEDURE:

• Calibrate a pH meter with buffer pH 4, 7 and 10

• Rinse the electrode with distilled water after calibration and dip the electrode into the

sample, stir and allow to stabilize.

• Record the readings on the pH meter as the value sample.

4.1.6 DETERMINATIONOF TOTAL DISSOLVED SOLID

METHOD: INSTRUMENTATION

PROCEDURE

• Rinse the TDS meter with distilled water and clean with a clean tissue.

• Dip the electrode into the sample.


• Record the readings on the TDS meter

4.2 PHYSICO-CHEMICAL ANALYSIS OF FOOD

4.2.1 DETERMINATION OF FAT CONTENT

This method is based on loss on drying of water and other volatile compounds at an oven

temperature of 1050C. It involves the measurement of the weight loss due to evaporation.

MATERIALS: Gottlieb tubes with siphons, conical flask, Beakers, Desiccators, a pair of

tong, Analytical Balance, Diethyl ether, Petroleum ether, Concentrated ammonia solution,

Ethanol, Water bath, Hot air oven, Spatula, Distilled water.

PROCEDURE:

• Dry the empty beaker in the hot air oven and cool in desiccators.

• Weigh the cooled empty beaker (W1).

• Weigh 2g sample into the Gottlieb tube and record the weight (W).

• Add 10ml of distilled water and warm in water bath to the weighed sample and mix

well.

• Add 2ml of concentrated ammonia. Mix the solution well and allow to cool.

• Add 10ml of ethanol and shake for 30 seconds.

• Add 25ml of Diethyl ether and cork the tube. Shake for 1 minute.

• Add 25ml of Petroleum ether and shake for 30 seconds.

• Insert siphon into the corked Gottlieb tube containing the mixture and blow the

ether of fat layer (through the siphon) into the pre-weighed beaker.
• Repeat the extraction two more times using 25ml of 1:1 both Diethyl ether and

Petroleum ether and 5ml of ethanol each time, siphon the extract into the

preweighed beaker.

• Place the extract in the beaker on a water bath at 100 oC to evaporate off the ether in

the fume cupboard.

• Transfer the beaker (containing the residue) into the oven at 105 oC for 30mins to

dry the extracted fat.

• Transfer to the desiccators to cool to room temperature, weigh and record the

weight of dish plus fat (W2).

Percentage % Fat content

4.2.2 DETERMINATION OF CRUDE PROTEIN

This method will not include nitrogen from nitrites and nitrates but will include nitrogen from

protein, alkaloids, etc. The organic matter is oxidized by concentrated sulphuric acid in the

presence of catalyst and the nitrogen converted to ammonium sulphate. This then made

alkaline and the liberated ammonia is distilled and estimated.

As a very large part of the nitrogen present in foods is derived from proteins, the crude protein is

estimated by multiplying the percentage of the nitrogen by an appropriate factor.

MATERIALS AND EQUIPMENT: Concentrated sulphuric acid-nitrogen free, NaOH

containing 5% Na2SO4 (sodium thiosulphate), boric acid, sulphuric acid, screened methyl red

indicator 0.016%, methyl red and 0.083%, bromocresol green in alcohol, kjeldal catalyst +

tablets containing

1g of Na2SO4 and 0.1g hydrated copper sulphate or

1g of Na2SO4 and 0.1g mecury, 1 gram of Na2SO4 AND 0.05g of selenium.


REAGENTS: 50% NaOH; Dissolve 5g of NaOH in distilled water and dilute with 100ml of

distilled water

Boric acid: 2g of Boric acid in distilled water and dilute with 100ml.

PROCEDURE:

• Weigh out a portion of the prepared sample equivalent to about 0.2g protein and transfer it

into a kjedahl digestion flask. If a filter paper is used for weighing, the sample may be

transfer into the flask with the filter paper. A similar paper must be used in the blank.

• Add 25ml of concentrated H2SO4 and 1 tablet of kjedahl catalyst or the alternative

formation to the flask.

• Heat the flask gently in and inclined position (if using a flame) in a fume hood until

frothing ceases (Anti foaming agents can be added)

• Then increase the heat and continue digestion until the liquid is clear and free from dark

color.

• Allow the flask to cool and dilute the content with about 200ml distilled.

• Add anti bumping granules to the flask

• Connect flask to a distillation apparatus incorporating and efficient splash head and

condenser.

• Measure out 50ml of boric solution into 250ml conical flask and add few drops of screened

methyl red indicator and place in on the receiver so that the end of the delivery tube from

the condenser dips just below the level of the boric acid.

• Close the apparatus


• Run in about 25ml of NaOH solution through the dropping funnel to make the liquid in the

flask distinctly alkaline.

• Mix the content of the digestion flask.

• Boil until at least 150ml have distilled into the receiver.

• Remove receiver with delivery tube, then remove the source of heat.

• Wash down the delivery tube into the receiver and titrate with 0.1M Hcl or 0.05M

H2SO4.

• 1ml of 0.1M hydrochloric acid or 0.5 w2 – w3M H2SO4= 0.0014Gn

%N =

W = weight of sample taken

% Protein = %N x F

4.2.3 DETERMINATION OF MOISTURE CONTENT

This is based on loss on drying of water and other volatile compounds at an oven temperature of

1050C. It involves the measurements of the weight loss due to evaporation.

MATERIALS: Evaporating dishes, desiccators, hot air oven, pair of tongs, forceps and analytical

weighing balance.

PROCEDURE:

• Clean and oven dry petri dish and cooled in a desiccator.

• Weigh the dish and record the weight of the dish (w1).

• Weigh about 5g into the evaporating dish and record (w2) and transferred carefully using a

forceps into the hot air oven at 1050C for 3 hours.


• Transfer the dish with sample after drying into the desiccator to cool and weigh on a weighing

balance (w3) is recorded.

• Evaporating dishes returned to the hot air oven for another 30 minutes, cool in the desiccator

and weigh again. This should be repeated until a constant weight is obtained and recorded as

final weight.

% Moisture content= x 100

4.2.4 DETERMINATION OF SPECIFIC GRAVITY

Specific gravity is a measure of how heavy a liquid is, compared to water. Specific gravity is thus

an inverse measure of a liquid’s density relative to that of water.

MATERIALS: 50ml pcynometer (specific gravity) bottle, distilled water, weighing balance.

PROCEDURE:

• Weigh a dry empty pcynometer (50ml) with lid and record.

• Fill the bottle to the brim with the sample and insert the lid in such a way that the sample flows

through it.

• Clean the spilled sample off the bottle, weigh and record value.

• Carry out the above procedure using the distilled water first before sample, both at the sample

temperature.

• Temperature is preferably at 200C.


4.2.5 DETERMINATION OF TITRATABLE ACIDITY

EQUIPMENT: Conical flask, measuring cylinder, pipette, retort stand, burette, distilled water,

water bath.

REAGENTS: 0.1M NaOH, Phenolphthalein indicator

PROCEDURE:

 Measure 5ml of the sample into a conical flask

 Place the sample measure in the conical flask on a water bath to evaporate dryness.

 Then add 10ml of the sample to evaporate again

 Put it out of the water bath to cool

 Add a pinch of phenolphthaline indicator.

 Add 25ml of distilled water to the mixture

 And then titrate with 0.1M NaOH against pink colour at the end point.

1m 0.1M NaOH = 0.006g acetic acid, 0.007g of lactic acid

T = Titre value

F = Factor

Acidity=

4.2.6 DETERMINATION OF ASH CONTENT

This method relies on burning off the organic component (in the sample) in the presence of air.

Residue consists of the inorganic components in form of their oxides.

MATERIALS: Crucibles, Muffle furnace at 5500C, Desiccators, a pair of tong, Analytical

Balance.
.

PROCEDURE:

• Ignite crucible at 550oC and allow it to cool in desiccators.

• Weigh the cooled empty crucible (W1).

• Weigh 2g test portion in crucible and record the weight (W).

• Transfer the crucible (containing the sample) into the muffle furnace to ash at 550 oC for 3hours

until ash is white and there is no dark particle in it.

• Transfer the ashed sample to the desiccators to cool, weigh and record crucible with sample

after ashing (W2).

% Ash = Weight of crucible and ash - Weight of empty crucible x 100

Weight of sample

% Ash = W2 – W1 x 100

Where: W = Weight of sample

W1 = Weight of empty crucible

W2 = Weight of crucible and ash

4.2.6 DETERMINATION OF ENERGY

APPARATUS: Crucible, Hot Plate, Spatula and Thong.

PROCEDURE:

 We measure or weigh the crucible before adding the sample.


 We measure 10g of the food sample inside the crucible.

 We then heat the food sample until it is red hot.

 We measure a suitable amount of water inside the beaker and check the temperature of the

water using a mercury in glass thermometer.

 After the food substance has been heated up we pour the food substances into the beaker

containing water and measure the temperature.

Energy=
CHAPTER FIVE

5.0 SUMMARY OF ATTACHMENT ACTIVITIES

This industrial training has afforded me the basic and practical knowledge that I may not have

gotten from the lecture room. It helped me to learn the importance of interacting with other

colleagues so as to achieve a common goal.

Finally, the SIWES training has helped to bridge the gap between academic theory and

practical and has built a degree of confidence in me on how knowledge can be converted to

action to help solve problems and meet human want.

5.1 PROBLEMS ENCOUNTERED DURING THE PROGRAM

 Getting SIWES placement within a short range of time.

Transportation in terms of finances from home to the place of training.


 Short duration of SIWES which limited total exposure to the plant operation.

5.2 SUGGESTION FOR IMPROVEMENT OF THIS SCHEME

Seeking placement for training should be made easy for much knowledge to be acquired.

Also, more time should be given for the period of the training.

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