intertek_internship_report

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TABLE OF CONTENTS

1.0. INTRODUCTION ................................................................................................................... 4

1.1 Internship Objectives............................................................................................................. 4

1.1.1. Objectives for the Company .......................................................................................... 4

1.1.2. Career Objectives .......................................................................................................... 4

1.1.3. Academic Objectives ..................................................................................................... 4

1.2. INTERNSHIP ORGANIZATION ........................................................................................... 5

1.2.1. Company’s Statements. ..................................................................................................... 5

Mission Statement ................................................................................................................... 5

Quality Statement .................................................................................................................... 5

The Company’s Core Values ................................................................................................... 5

Company’s Motto .................................................................................................................... 6

1.2.2 Administration Hierarchy ................................................................................................... 6

2.0. GENERAL PROCESSES AT INTERTEK ............................................................................. 7

2.1 Laboratory Services............................................................................................................... 7

2.1.1 Petroleum Laboratory ..................................................................................................... 7

2.1.2. Agriculture Laboratory .................................................................................................. 7

2.1.3. Microbiology Laboratory. ............................................................................................. 8

2.2. Environmental Impact Assessments (EIA) and Environmental Audit (EA) Services ......... 8

2.3. Inspection Services ............................................................................................................... 8

3.0 TESTS IN PETROLEUM LABORATORY ............................................................................ 9

3.1. Tests of Density and Relative Density of Petroleum Products and Chemicals .................... 9

3.1.1 Determining Density Using Digital Density Meter (ASTM D4052) ............................. 9

3.1.2. Determining density and Relative Density Using Hydrometer (ASTM D1298 .......... 12

3.2. Determining kinematic viscosity at 400C, 50

0C and 100

0C (ASTM D445-06) ................. 14

3.3. Determining The Flash Point Of Petroleum Products (ASTM D93 And IP 170) ............. 17

3.4. Manual Distillation of Petroleum Products at Atmospheric Pressure (ASTM D86) ......... 18

3.5. Doctor Test (IP 30) ............................................................................................................. 20

3.6 Determination Of Mercaptan Sulphur Using Titrino .......................................................... 21

3.7. Determining Asphaltene Content In Petroleum Products (IP 143) ................................... 25

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3.8. Determining The Total Sulphur Content ( D4294) And Total Lead Content (IP 352)

Using X- Ray Fluorescence (XRF) ........................................................................................... 26

4.0. Quality Control during Analysis ............................................................................................ 28

4.1. Daily Monitoring Of Ambient Conditions ......................................................................... 28

4.2. Carrying out Blank Tests.................................................................................................... 28

4.3. Quality Control Samples (QC) and Quality Control Measurements.................................. 29

4.4. Calibration of Instruments .................................................................................................. 29

4.5. Use of Standard Methods, or Validated in-house Methods ............................................... 29

4.6. Proficiency Testing (PT) Participation ............................................................................... 29

4.7. Internal And External Audits ............................................................................................. 30

5.0. HEALTH, SAFETY, SECURITY AND ENVIRONMENT (HSSE) ................................... 31

5.1.Training of Personnel .......................................................................................................... 31

5.2.Provision of Personal Protective Equipment (PPE) ............................................................ 31

5.3.Provision of Material Safety Data Sheet (MSDS) .............................................................. 31

5.4.Environmental Management ............................................................................................... 32

5.4.1.Solid waste products......................................................................................................... 32

5.4.2.Liquid Waste Products ..................................................................................................... 32

5.4.3.Gaseous Waste Products .................................................................................................. 32

5.5.Control Of Pollution ............................................................................................................... 33

5.5.1.Use of fume chambers, muffles and fume extractors ....................................................... 33

5.5.2.Collection Of The Slopes And Safe Discharge ................................................................ 33

5.5.3.Solid Wastes Collection ................................................................................................... 33

5.5.4External And Internal Audits ............................................................................................ 33

5.5.5.Constant Employee Training ............................................................................................ 33

6.0. Recommendations .................................................................................................................. 34

6.1. Introduction of Marketing Department. ............................................................................. 34

6.2. Revenue Generation from Retained Samples..................................................................... 34

6.3. Introduce Ron and Induction Methods ............................................................................... 35

6.4. Quality Control Adjustments. ............................................................................................ 35

6.5. Position and Working of the Thermometers ...................................................................... 35

6.6. Corrosion of Expensive Instruments .................................................................................. 35

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6.7. Quality Control on the Balances, And Special Positioning. .............................................. 36

6.8. Provision of full Personal Protective Equipment (PPEs) for the Attachees ....................... 36

7.0. References .............................................................................................................................. 37

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1.0. INTRODUCTION

1.1 Internship Objectives

Being my first internship experience, I wanted to maximize on the three months hence set clear

objectives which I analyzed weekly to measure my progress and work on the perceived

weaknesses.

1.1.1. Objectives for the Company

Be able to perform at least three new tests each week so as to take part in the daily

laboratory activities.

Understand the company’s culture, core values by analyzing the company’s mission,

vision and quality statements as well as its goals and objectives.

Study the management system to find out why Intertek experiences a steady growth in

popularity in the industry, and how as a potential employee I can better its growth in the

market.

By the end of the internship period, produce a timely and comprehensive report to the

Laboratory manager. This will be through daily collection of necessary information.

1.1.2. Career Objectives

Gain professional, interpersonal and communication skills by constant practicing,

understanding the behaviours of my colleagues and clarifying instructions before

executing assignments

Networking through exchanging contacts, socializing with people and sharing

experiences.

Be a potential candidate for future or current job opportunities by displaying

professionalism and open-mindedness in the way I carry out designated tasks.

1.1.3. Academic Objectives

Complete the Industrial Attachment Unit (SCH 321) by completing the three months

offered

Be ready for the assessment by the university supervisor by exhaustively filling my

practicum logbook, and having a wide knowledge of the laboratory activities.

Compile a comprehensive internship report as required by the Faculty of Chemistry.

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1.2. INTERNSHIP ORGANIZATION

Intertek Testing Services is an international proprietary company with over six hundred offices

and laboratories worldwide. Intertek Kenya has its main office in Mombasa at David Keyanda

Road, Kizingo. Founded in 1994, it offers services such as laboratory, environmental Impact

assessment and environmental audit as well as Inspection and certified for IS0 9001:2008.

1.2.1. Company’s Statements.

Mission Statement

“Our mission is to add value for our customers by helping them achieve their desired level of

quality and safety for their products, assets and processes; to protect their brands and enable their

success in the global marketplace. “

Quality Statement

Intertek states its intention to establish, implement and maintain a quality management system

designed to ensure that services undertaken are fit for their intended purposes in line with IS0

9001:2008. Further, the company states its commitment to meeting and exceeding customer

stated and implied needs through a process of continual improvement.

The Company’s Core Values

“Our commitment to supporting and adding value for our customers drives everything we do.

We deliver innovative solutions to facilitate our customers’ success in the global marketplace

and, most importantly, we provide our customers with confidence.

By leveraging our local service and global network, we enable our customers to dedicate their

primary energies to their core business activities. We offer comprehensive programmers and

services which draw on our industry specific knowledge and technical expertise.

At Intertek, and as individuals, we:

Value trust and personal responsibility;

Act with integrity, honesty and respect;

Maintain professionalism and strive for continual improvement and innovation;

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Deliver excellent services which add value to our customers’ business;

Focus on continual growth and outstanding performance;

Strive to create a safe work environment;

Value each employee’s contribution toward achieving our business objectives;

Promote a culture where motivated customer-oriented employees can flourish, experience

professional fulfillment, and reach their highest potential; and

Respect diverse perspectives, experiences and traditions as essential.

Our commitment to delivering outstanding results through sound and thorough financial

practices, superior profitability, stable growth and good citizenship will enable us to fulfill

Intertek’s mission while increasing sustainable shareholder value.”

Company’s Motto

The company’s motto is: Valued Quality. Delivered.

1.2.2 Administration Hierarchy

Regional Manager-Southern & Easter Asiia

Country Manager

Inspection Department

Operations Manager- Agri

Supervisors

Surveyors

Operations Manager- Petr

Surveyors

Laboratory Departments

Lab Manager

Lab supervisors

Lab technicians

Lab assistants

Admin Department

Office Admin Coordinator

Office Admin Assistants

Office Assistants

Human resource Manager

Admin Assistants

Office Assistants

Environmental Department

Env Manager

Env Auditor

Compliance Dep

Compliance Manager

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2.0. GENERAL PROCESSES AT INTERTEK

2.1 Laboratory Services

Equipped with modern facilities, the laboratory department consists of three laboratories:

Petroleum, Agriculture and Microbiology. The services receive recognition from National

Environmental Management Authority (NEMA), accreditation for ISO/IEC 17025:2005.

To ensure the results are precise and accurate, the department participates in proficiency testing

organized by the Kenya Bureau of Standards, east African Bureau of Standards, South African

Bureau of Standards, FOSFA and GAFTA.

2.1.1 Petroleum Laboratory

The Petroleum Laboratory carries physical (density, viscosity, flashpoint, color) and chemical

(Total Acid Number, Asphaltenes) analysis as per approved and acceptable standards such as

KEBS) on petrochemicals and chemicals.

The common petroleum samples include: Heavy Fuel Oils (HFO), Automotive Gasoil (AGO),

Motor Gasoline (Mogas), Jet A-1 and Lubes. The chemicals include: Xylene, toluene, hexane,

coradol, and Low Aromatic White Spirit (LAWS).

The most important clients are Total Kenya, Magadi Soda, Galana Oil, Vivo Energy, Addax

Kenya, Haller Petroleum and Solvochem.

2.1.2. Agriculture Laboratory

Carries full analysis on agricultural and food samples as per local, international, IS0 3720,

destination and even clients requirements.

Analysis is on the moisture content, free fatty acids, protein content amongst others. The most

common samples include tea, leaves, coconut and vegetable oils, sesame, cloves and macadamia

nuts. The most important clients include: World Food Program (WFP), Export Trading. PISU

Company Limited, Louis Dreyfus Commodities, Unilever Kenya Limited and Cargill Kenya

Limited.

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2.1.3. Microbiology Laboratory.

Carries full analysis on the chemical, physical and microbiological analysis on food, water and

effluents as per the local (KEBS and NEMA) as well as international (WHO and ISO). The

analysis cover aflatoxin levels, Total Plate Count, and Total Coliform Count

Major clients include Baobab Beach Resort, JZEC Constructors, East African Packaging

Industries, GAPCO, World Food Program and African Marines.

2.2. Environmental Impact Assessments (EIA) and Environmental Audit (EA) Services

Introduced in 2012, the department offers environmental services to its clients independently

according to local standards and the provisions of the Environmental Management and

Coordination Act, 1999 and Environmental Impact Assessment and Audit Regulations, 2003 as

administered by the National Environmental Management Authority (NEMA)

The Services include environmental auditing and technical services and customer

recommendations for environmental operations.

2.3. Inspection Services

Provides inspection of systems, processes and products as per relevant international and local

standards. The Inspection department contains two major sections: Agriculture (commonly

called Veg by the inspection team) and Petroleum. The quality of service delivered is ensured by

the certification for ISO/IEC 17020:2005.

The scope of work covers the inspection of: containers prior to stuffing, tally bags during

stuffing; weighing 10% of cargo during stuffing, noting bag marks and or any abnormalities;

container sealing after stuffing, fumigation witnessing; sampling and taking digital photographs.

This department is also important to the company as it markets the laboratory department by

carrying out analysis for its clients. As it can be seen, most of its clients are also clients of

laboratory department: WFP, East African Storage, Export Trading Company and PISU

Company Limited.

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3.0 TESTS IN PETROLEUM LABORATORY

Included in this section are the tests that I was able to carry out during my one and a half months

of internship, and not necessarily all the tests available in the laboratory. They are all in a

summarized format, concentrating mainly on the working principles of the instruments involved

(if any) and their significance. Quality control involved in the tests as well as recommendations

is dealt with separately.

3.1. Tests of Density and Relative Density of Petroleum Products and Chemicals

Density is mass per unit volume. In the laboratory, density measurements are taken at using two

methods, the reference method (ASTM D1298) and the use of a digital density meter (ASTM

D4052). Density being a function of temperature, its measurements are determined at 20⁰C

(ASTM D4052) or corrected to 20⁰C (ASTM D1298).

3.1.1 Determining Density Using Digital Density Meter (ASTM D4052)

An Overview of the Instrument

The density meter used is a DMA M series of 4100 manufactured by Anton Paar. The

measurement is based on the oscillating U-tube method which was invented by Dr. Hans

Stabinger and Dr. Hans Leopold at the Joanneum Research Institute (Graz, Austria) and first

introduced onto the market by Anton Paar in 1967.

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A major source of measuring errors when using density meters are gas bubbles in the measuring

cell. This issue was addressed by Anton Paar with two new features:

• FillingCheckTM

: The instrument automatically detects inhomogeneities and gas bubbles in the

whole measuring cell by an advanced analysis of its oscillation pattern and generates a warning

message in real time for any single measurement.

• U-ViewTM

: You can visually inspect the measuring cell using a real-time camera with zoom

function (DMA 4500/5000 M).

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The Working Principle

The sample is introduced into a U-shaped borosilicate glass tube that is being excited to vibrate

at its characteristic frequency. The characteristic frequency changes depending on the density of

the sample. Through a precise determination of the characteristic frequency and a mathematical

conversion, the density of the sample can be measured. The density is calculated from the

quotient of the period of oscillations of the U-tube and the reference oscillator:

Density Ka× Q× f1- Kb × f2

Where:

Ka, Kb Apparatus constants

Q Quotient of the period of oscillation of the U-tube divided by the period of oscillation of the

reference oscillator

f1, f2 Correction terms for temperature, viscosity and nonlinearity

Apparatus|Reagents

DMA 4100

Cleaning Solvent (toluene)

Distilled water for calibration

Syringe

Preparation

The equipment is turned on and allowed to stabilize for at least 20 minutes. However, the

common practice is to leave it on overnight, connected to a UPS to prevent any deviations

resulting from power fluctuations. Cleaned by toluene, it is purged with acetone for drying and

the humidity levels read from the nearby hygrometer to check if it is within the required limits

(covered under quality assessment)

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Procedure

The sample, after being homogenized by vigorous agitation and ensuring there are no air

bubbles, is put in a syringe and introduced into the sample. The measure button is pressed, and

the density taken after duplicate measurements. The duplicate measurements should not differ by

more than 0.0002kg/l. If they do, discard both measurements and repeat the procedure.

Report the density displayed in g/cm3, kg/l or kg/m

3, correct to four significant figures.

3.1.2. Determining density and Relative Density Using Hydrometer (ASTM D1298)

This is the reference method for density calculation of petroleum products as well as chemicals

normally handled as liquids and having a Reid Vapor pressure of 101.25kPa or less, using a glass

hydrometer.

Apparatus| Reagents

Hydrometers

Hydrometer Cylinders which should be clear glass, plastic or metal. The inside diameter

should be at least 25mm greater than the outside diameter, and when immersed in the

liquid, at least 25mm of the hydrometer floats on it. Those of plastic nature should not be

affected by the sample, nor gets discolored by exposure to light.

Thermometers whose allowed range is between -10oC to 38

oC and -20

oC to 102

0C. They

should undergo verification at intervals of not more than six months for conformance and

specifications.

Constant temperature bath if required, of dimensions such that it can accommodate the

hydrometer cylinders comfortably during measurement and maintain the temperature of

the water within 0.250C of the test temperature.

Stirring Rod of glass or plastic of approximately 400mm. A liquid –in glass thermometer

can be used.

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Procedure

The homogenized, air-free sample is brought to the test temperature (normally 50oC), and

transferred into a temperature stabilized thermometer placed in a vertical position. The liquid is

stirred using a thermometer, the temperature recorded and the hydrometer reading noted as

below:

.

The meniscus correction is then applied, a duplicate measurement made if the temperature

difference differed from the original by 0.050C. Relevant thermometer corrections are made from

the calibration certificate, and the final value reported in kg/l at the reference temperature to the

nearest 0.0001kg/l.

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Importance of Density

The measured value can be used to convert volumes of the petroleum products or

chemicals into masses; which is very important in offloading and transport of these

products from ships to outlets as well as during selling

An important quality, when correlated with other factors, considered during pricing of

petrochemical products

An important quality indicator for automotive fuels during storage, handling and

transportation.

For the analysts, these quotes will suffice to demonstrate the importance of ensuring accuracy

and precision in determining density:

“We have lost client(s) because of density,” the Quality Manager, during my

induction process.

“Because of difference in the last three digits, 630 liters have been lost,” Mr

Kuteli, the Operations Manager for Petroleum, when the theoretical density

differed from the practical one by some few digits.

3.2. Determining kinematic viscosity at 400C, 50

0C and 100

0C (ASTM D445-06)

The viscosity of a fluid is a measure of its resistance to gradual deformation by shear or tensile

stress. It is a fluidic property resulting from collisions between neighboring particles in a fluid

that are moving at different velocities. Two types of viscosities are of interest: dynamic and

kinematic viscosities.

Dynamic viscosity, also called dynamic viscosity, is the tangential force per unit area required to

move one horizontal plane with respect to another plane, at a unit velocity, when ,maintaining a

unit distance apart in the fluid. Kinematic viscosity, on the other hand, equals the ratio of

absolute viscosity to the density. Its SI unit is the Stoke (St). A Stoke equals one square meters

per second:

1 Stoke m2/s

Since the Stoke is a very large unit, smaller units such as the centistokes (a hundredth of a

Stoke) are normally used. Other local units are the Engler, Saybolt and Redwood. They are all

interconvertible.

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Measurement of Viscosity.

Viscosity is measured using viscometers, also called rheumeters. These viscometers have

designated numbers, with corresponding coefficients. Measuring viscosity is determined by the

tangible force required to displace the materials particles with a specific deformation-flow i.e.

velocity. The relationship between the tangible force and the deformation flow obtains the

viscosity result. Ambient conditions such as temperature and pressure also have an effect on

viscosity. Because of this, the viscometer is immersed in an oil bath kept at a constant

temperature using an intrinsic thermostat. The time taken for the fluid to move between the two

meniscuses should be between 200-1200 seconds.

Types of Viscometers

An important accessory is the viscometer holder, which can take different designs depending on

the viscometer type:

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Apparatus | Reagents

Calibrated Viscometer

Viscometer holder

Calibrated thermometer

Calibrated stop watch

Sucker

Cleaning solvent (toluene-acetone mixture)

Preparation and Procedure.

The bath is switched on to attain the required temperature, ensuring the viscometer is clean and

dry. After being charged to the filling mark, the viscometer is allowed to attain the test

temperature for at least 30 minutes. Removing the fitting on the viscometer, pressure allows the

fluid sample to flow freely, and the time between the two meniscuses recorded. A duplicate

result is obtained by repeating the procedure.

Calculation and Reporting

The Kinematic viscosity (σ) is obtained using the following formula:

σ k × t, where:

k he viscometer constant (mm/s2)

t time taken by the fluid to fklow between the two meniscuses

σ kinematic viscosity in mm/s

Importance Of Kinematic Viscosity

Knowledge of the kinematic viscosity of the sample is important in determining its ease

of flow, hence its ease of transportation from one installation to another

It is a characteristic quality of oil, hence needed in quality assessment especially in

determining whether it has been mixed with other oils

Being affected by the density of the oil, viscosity can be correlated to volume in the

calculation of the mass of the sample, especially during pricing.

Where the petroleum product is used as a lubricant, viscosity becomes important in the

efficiency of the lubrication.

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3.3. Determining The Flash Point Of Petroleum Products (ASTM D93 And IP 170)

Flash point, in petroleum products, the lowest temperature corrected to a barometric pressure of

101.3 kPa (760 mm Hg), at which application of an ignition source causes the vapors of a

specimen of the sample to ignite under specified conditions of test. The test specimen is deemed

to have flashed when a flame appears and instantaneously propagates itself over the entire

surface of the test specimen. When the ignition source is a test flame, the application of the test

flame may cause a blue halo or an enlarged flame prior to the actual flash point. This is not a

flash point and shall be ignored.

Normally carried out in two different apparatuses; Abel Closed Cup (manual or semi-automated)

and Pensky Martens Closed Cup. The latter is used for samples such as fuel oils, gasoline and

lubes, while the former for Jet A-1 and illuminated Kerosene (IK).

Summary of Test Method

A brass test cup of specified dimensions, filled to the inside mark with test specimen and fitted

with a cover of specified dimensions, is heated and the specimen stirred at specified rates, by

defined procedures. An ignition source is directed into the test cup at regular intervals with

simultaneous interruption of the stirring, until a flash is detected as explained above and the

flashpoint reported from the thermometer when a flame appears and instantaneously propagates

itself over the entire surface of the test specimen.

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Importance Of The Flash Point

The flash point temperature is one measure of the tendency of the test specimen to form a

flammable mixture with air under controlled laboratory conditions. It is only one of a

number of properties which must be considered in assessing the overall flammability

hazard of a material.

Flash point is used in shipping and safety regulations to define flammable and

combustible materials. One should consult the particular regulation involved for precise

definitions of these classifications.

Also used for detecting contamination of relatively non-volatile or non-flammable matter

used to measure and describe the properties of materials, products, or assemblies in

response to heat and an ignition source under controlled laboratory conditions.

3.4. Manual Distillation of Petroleum Products at Atmospheric Pressure (ASTM D86)

This test method covers the atmospheric distillation of petroleum products using a laboratory

batch distillation unit to determine quantitatively the boiling range characteristics of such

products as natural gasoline, light and middle distillates, automotive spark-ignition engine fuels,

aviation gasoline, aviation turbine fuels, I-D and 2-D regular and low sulfur diesel fuels, special

petroleum spirits, naphthas, white spirits, kerosines, and Grades 1 and 2 burner fuels.

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Apparatus Arrangement

Summary of Test Method

Based on its composition, vapor pressure, expected initial boiling point or expected final boiling

point, or combination thereof, the sample is placed in one of five groups. Apparatus arrangement,

condenser temperature, and other operational variables are defined by the group in which the-

sample falls, according to ASTM D 86 clause 3.1.1 A 100-mL specimen of the sample is

distilled under prescribed conditions for the group in which the sample falls.

The distillation is performed in a laboratory batch distillation unit at ambient pressure under

conditions that are designed to provide approximately one theoretical plate fractionation.

Systematic observations of temperature readings and volumes of condensate are made,

depending on the needs of the user of the data. Mostly, it is the initial boiling point, and the

temperatures at the recoveries of the volumes at 10%, 20%, 50% and 90%. The volume of the

residue and the losses are also recorded

For highly volatile samples such as mogas, chilling before distillation is required, and the

distillate collected in a c very cold environment such as ice-cold water. When the data is

collected, the thermometer readings are corrected using the calibrations standards as well as

barometric pressure corrections.

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Importance of the Distillation values obtained

The distillation (volatility) characteristics of hydrocarbons have an important effect on

their safety and performance, especially in the case of fuels and solvents. The boiling

range gives information on the composition, the properties, and the behavior of the fuel

during storage and use.

Volatility is the major determinant of the tendency of a hydrocarbon mixture to produce

potentially explosive vapors. Volatility, as it affects rate of evaporation, is an important

factor in the application of many solvents, particularly those used in paints.

The distillation characteristics are critically important for both automotive and aviation

gasolines, affecting starting, warm-up, and tendency to vapor lock at high operating

temperature or at high altitude, or both. The presence of high boiling point components in

these and other fuels can significantly affect the degree of formation of solid combustion

deposits

Distillation limits are often included in petroleum product specifications, in commercial

contract agreements, process refinery control applications, and for compliance to

regulatory rules.

3.5. Doctor Test (IP 30)

This is a qualitative test for determining the presence of mercaptan sulphur in petroleum

products, especially Jet A-1. Mercaptan sulphur, also called thiol, is an organosuphur that

contains a carbon-bonded sulphhydrl (C- SH or R-SH). It is responsible for the characteristic

garlic smell in some petrochemicals, and is normally used as odorants in the detection of natural

gas.

The test aims at attacking the thiol group through introduction of lead into it, and then

precipitating the lead as a salt by reacting with sulphur flowers:

NaPbO2 2 R-SH (RS)2Pb 2NaOH

(RS)2Pb S RS-SR PbS

A sample is said to be Doctor sweet if it fails to produce a dark precipitate of lead sulphide.

Apparatus| Reagents

100 ml of measuring cylinder

Sulphur flowers

Sodium plumbite solution

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Spatula

Preparation of Sodium plumbite solution

Dissolve 25g of lead acetate trihydrate in 200ml of water . filter and add to a solution of 60g of

NaOH in 100ml of water. Heat the mixture in a boiling water bath for 30 minutes, cool and dilute

to 1000ml of water.

Procedure And Reporting

10 ml of sample is poured into a cylinder followed by 5ml of sodium plumbite solution, the

cylinder closed with a stopper. The cylinder is shaken vigorously for 15 seconds, and let to settle

while observing the interphase. After adding a small quantity of sulphur flowers, the solution is

shaken for 15 more seconds and the content of the cylinder carefully observed.

If a black precipitate is formed, the test is reported as being positive. Otherwise, negative.

Importance of test

It is a good prerequisite for the Mercaptan Sulphur test using Titrino

The content of sulphur in an oil sample ( whether chemically bonded or physically

contaminated) is important since the it is guided by local and international standards

3.6 Determination Of Mercaptan Sulphur Using Titrino

This instrument determines the quantitatively the amount of mercaptan sulphur present in a

sample by potentiometric means. The sample is mixed with a titrating solvent, stirred

vigorously and its potentiometry correlated with the concentration of mercaptan sulphur.

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Overview of the Instrument

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Preparation And Filling Of The Titrating Solvent

1.6g of sodium acetate is added to 20ml of deoxygenated distilled water and the solution

mixed with 975ml of isopropyl alcohol followed by addition of 4.6g of glacial acetic acid.

During filling of the titrating solvent, it is important to ensure it is thoroughly mixed by

ensuring the stirred is placed centrally; and oxygen free by regulating the stirring speed

(should not be too high)

Operating The Instrument And The Procedure

Weigh approximately 30g of the sample in the glass beaker and then add 100ml of

acidic titrating solvent and place it in the equipment.

Press power button on

When the menu windows appears, fill where appropriate then select MERCAPTAN,

then press OK

On the method table window, press START

Run your sample then read and record the value displayed.

The machine is switched off, and the electrode is stored in distilled water.

3.7. Determining Asphaltene Content In Petroleum Products (IP 143)

This method describes the quantitative determination of asphaltenes; those hydrocarbons

insoluble in heptane but soluble in hot benzene/toluene. The sample is first dissolved in heptane,

and the residue filtered through a filter paper then the filter paper refluxed in the filtrate to

remove any undissolved matter. The filter paper is then refluxed in hot toluene to dissolve all the

asphaltenes, and their content determined mathematically.

Procedure

Weigh 3-5g of the sample followed by addition of 30ml of heptane per gram of the sample. Boil

the mixture under reflux for an hour, then cool and store the content of the flask for about 2

hours. Filter the content of the flask in another flask using grade 42 filter paper, and keep the

original flask aside for later use. Extract the content of the filter paper under reflux with heptanes

for at least an hour, followed by extraction with toluene in the original flask under reflux. Put the

content of the flask in a pre-heated (1050C for 30 minutes ), cooled and weighed. Wash the flask

completely with at most 30ml of toluene. Evaporate the toluene in a water bath. Dry the dish,

cool and weight.

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3.8. Determining The Total Sulphur Content ( D4294) And Total Lead Content (IP 352)

Using X- Ray Fluorescence (XRF)

Working Principle

when a sample containing an element A is irradiated by a primary X-ray, the intensity of the

generated fluorescent X-ray of element A is dependent on its fraction in the sample. The higher

fraction of element A in the sample, results in a higher intensity of the fluorescent X-ray that is

generated. Taking this into account, the volume fraction of certain element can be determined

knowing the respective fluorescent X-ray intensity.

The Source of the X-rays

The above figure is an illustration of an X-ray tube. For our X-ray, the coolant was a fan driven

by a motor instead of water to yield higher cooling efficiency. A thin beryllium (highly

transparent to X-rays) window is used that certain X-rays can escape the shielded X-ray tube

towards the sample. The X-rays from the cathode are produced as a result of thermionic

emissions of electrons, which when accelerated towards the anode, sudden stoppage results in

the emission of X-rays.

In general, a quantitative XRF analysis can be conducted using a standard curve. This method

involves measuring several samples with a known element concentration, and finding the

relationship between the intensity of the measured element's fluorescent X-ray and the

concentration. By referring this relationship, element concentration of unknown sample is

obtained only with information on its fluorescent X-ray intensity.

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Sample Preparation and Instrument Operation

The sample is put in a sample cell up to the mark indicated; at least three-quarters full. Then a

standard is obtained for that particular sample and the corresponding test. The sample is inserted

into the XRF, (when the radiation source is turned off), then the text selected from the menu. The

standard is then inserted, and the obtained value is used to correct any deviation that might have

been experienced during the test.

Importance of Determining the Lead Content

Lead is a pollutant, causing various respiratory disorders and is also carcinogenic

There are local and international standards regarding the minimum allowable

concentration of the lead content in a fuel.

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4.0. Quality Control during Analysis

Quality control is the sum processes of ensuring that the procedures of analysis and the

environmental conditions, as well as all the factors that affect the analysis are as per the set

standards. This is in agreement with the company’s motto: Valued Quality. Delivered.

There are many ways that are used to control quality in the laboratory and analysis in general,

such as:

4.1. Daily Monitoring Of Ambient Conditions

This refers to recording of the prevailing temperature, pressure and relative humidity in the labs

in the mornings and evenings, during the working days. There are wall thermometers installed in

all the three laboratories to monitor temperature, a hygrometer in the petroleum laboratory to

monitor relative humidity as well as a barometer for atmospheric pressure.

The monitoring is of significance since:

It is a requirement of ISO 17025:2005 and will be considered during audits to renew the

certification

These ambient conditions affect the results obtained. Distillation temperatures undergo

barometric corrections; density is affected by both temperature and humidity to a very

large extent.

It is a among the good laboratory practice for any ISO certified laboratory.

Failure to monitor may lead to audit failure.

Temperature and humidity have allowable ranges within which the environment is considered

safe for analysis. Normally, temperature is allowed to deviate between 20oC – 25

oC. Humidity

has limits for particular temperatures; at 20oC, it is supposed to range from 70oC-90

oC. Pressure

has no set limits, since it is not expected to vary greatly.

Apart from the laboratories, the sample store for petroleum laboratory also has the monitoring of

temperature since it affects the storage stability of the products, especially the more volatile.

4.2. Carrying out Blank Tests.

A blank reagent is the one containing all the constituents of the sample received except the

analyte of interest. Blank tests are used to cater for any impurities that might exist in the

commercial or prepared reagents that might have significant impact to the final results. This has

a way of ensuring that the final result has the required precision and or accuracy

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4.3. Quality Control Samples (QC) and Quality Control Measurements.

Quality control samples are samples of known concentration or known characteristics (such as

density or flashpoint) that are provided to the laboratory by trusted clients. They are used side-

by-side with the received samples to cater for any deviations, especially when instruments are

involved and largely relied in analysis. The readings given out by the instrument for the QC

sample can be used to:

Correct the deviation created by the instrument using a simple mathematical principle of

direct proportionality

Give account on the performance of the instrument and the analyst, especially for those

QC analyses done after every ten runs.

4.4. Calibration of Instruments

Calibration ensures that the readings given by the instruments are accurate, and this is done

constantly since deviations occur all the time. Calibrations can either be done by the trained

laboratory technicians themselves or externally by professional bodies. The former can be done

as often as the instrument requires; the latter annually or as per the instrument requirement.

4.5. Use of Standard Methods, or Validated in-house Methods

The laboratory uses internationally and locally accepted standard methods, such as those of:

American Standards of Testing and Materials (ASTM), Institute of Petroleum (IP), Kenyan

Bureau of Standards (KEBS), East African Bureau of Standards (EABS), amongst others. This

ensures quality deliverance of service, as well as compliance to client requests since some might

require other international standards.

In case where the analyst realizes another slightly different procedure that will yield same results

but with lower amount of energy (such as heating for 6 hours instead of 12) or overall cost, the

method is tested and validated, after which it is incorporated into the daily methods of analysis.

This not only shows competence of the analysts, but of the company as well.

4.6. Proficiency Testing (PT) Participation

Proficiency testing determines the performance of individual laboratories for specific tests or

measurements and is used to monitor laboratories’ continuing performance.

Proficiency testing is also called interlaboratory comparison. As this term implies, proficiency

testing compares the measuring results obtained by different laboratories.

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In a proficiency test one or more samples are sent around between a number of participating

laboratories. Each laboratory measures the artifacts (e.g. a ring gage or a set of gage blocks)

according to a given set of instructions and reports its results to the administrator.

The results reported by each laboratory for a measurement are compared to the reference value

for that measurement. The reference value can be determined in various ways. The two most

common ways are to use a reference laboratory or use the average of the values reported by the

participants. After results are collected, the zero score for each laboratory is determined and

results released.

4.7. Internal And External Audits

The company runs internal audits just before the external to monitor its performance as well as

upgrade its competence. Theses audits make it possible to scientifically determine the areas of

weakness or negligence and take proper action.

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5.0. HEALTH, SAFETY, SECURITY AND ENVIRONMENT (HSSE)

This is a separate departmental responsibility that is managed by the compliance manager. Its

main task is to ensure that the employee is provided with a highly conducive environment with

minimum health, safety and security risks. The procedures include:

5.1.Training of Personnel

Intertek has so far trained eight fire marshals and six first aiders. This ensures that the employees

are able to react quickly to emergency situations such as fire outbreaks or injury of employees.

5.2.Provision of Personal Protective Equipment (PPE)

PPE is all equipment (including clothing for protection against the weather) which is intended to

be won or held by a person at work and which protects them against one or more risks to their

health or safety. The table below summarizes the full set of PPE and the area of protection.

Number Area of protection Type of PPE

1 Whole body Overalls, chemical suites, lab-coats

2 head helmets

3 eye Safety glasses, goggles, face shields,

visors

4 feet Safety shoes, gum-boots

5 Hands Gloves

6 Ear Ear muffs, ear plugs

7 Drowning Life jackets

8 Respiratory Breathing apparatus, full face masks

9 Gases Personal gas monitors

10 Falling from heights Safety harness

11 fire Fire blanket

The PPE is given to the employee during his/her induction period, and is replaced annually.

Importance of PPE includes:

It is the last resort in risk control

It offers direct protection from hazards such as noise induced hearing loss, spillages and

crush or impact

The correct use of PPE prevents incurring of injury

Injuries incurred while wearing correct PPE are insured by the company. Those incurred

without are not, and may lead to loss of job.

5.3.Provision of Material Safety Data Sheet (MSDS)

MSDS is a document that contains the information on all the chemicals handled in the

laboratory, their hazards and the correct handling procedure. This gives a guide in case of major

or minor chemical spill or leak. It also assesses the extent of risk when an employee comes into

contact with these chemicals.

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Examples of harmful chemicals used include: xylene, benzene, chemical samples and reagents.

5.4.Environmental Management

As functioning laboratories, many waste materials are handled and/or released to the

environment. These wastes are classified into: solid, liquid and gaseous wastes.

5.4.1.Solid waste products

Their source in the petroleum laboratory are traced back to; residues of burnt oil products from

determination of total ash content, determination of total particulate matter of jet fuels, and from

the determination of asphaltene content. They primarily consist of minerals, dust particles as well

as carbon residues.

From the microbiology laboratory, these consist of damaged samples, residues of filtration

processes, and total ash content determination. They consist of damaged/expired cereal products

such as wheat or other food products, ashes, solid particles and damaged grains.

5.4.2.Liquid Waste Products

These consists of retained effluent samples such as sewage water, contaminated water (maybe

after oil spill), water used to wash and clean apparatus, as well as slopes ( remains of oil samples

collected in tanks)

5.4.3.Gaseous Waste Products

These are mainly products of combustion and consists of largely carbon (IV) oxide gas, activated

carbon particles (due to high temperatures of up to 750oC), as well as little amounts of sulphur

oxides and nitrogen oxides.

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5.5.Control Of Pollution

5.5.1.Use of fume chambers, muffles and fume extractors

Whenever burning or reflux extraction is required, it is done in fume chambers to ensure that the

fumes are extracted and pretreated before they are released into the atmosphere. The quantities

of these fumes are within the approved limits of NEMA.

Muffles with fume extractors are used for burning at higher temperatures, those ranging between

550oC-750oC. These ensure that no harmful fumes or smoke are released into the immediate

environment.

5.5.2.Collection Of The Slopes And Safe Discharge

The petroleum products which have been used are collected in tanks called slopes. These are

then safely discharged through a NEMA-certified client. Also, it is not allowed to pour oil

products into the sinks since theses sinks go directly to the ocean.

5.5.3.Solid Wastes Collection

The solid waste is collected in one container, and when filled, it is collected by the City Council

of Mombasa for safe discharge.

The company has ensured that the employees understand the wastes produced and handled in the

daily activities, as well as the impacts these wastes have in the environment. It has put certain

activities in place to constantly remind them, such as:

5.5.4External And Internal Audits

These are to ensure that the procedures for waste management are closely followed, detect any

deviations and take proper corrective actions.

5.5.5.Constant Employee Training

The employees undergo training on issues concerning environment and climate change, how the

company affects the environment and how to minimize its negative impacts.

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6.0. RECOMMENDATIONS

After being attached in the laboratory department for three months, I observed areas that need

improvement and thus recommend them here. These observations are not solely my own, some

of them are from the analysts I interacted with or during the meetings attended. They cover areas

such as management, quality control, increase of service delivery rate and methodologies.

6.1. Introduction of Marketing Department.

One of the aims of the company is to become the leading expert in the service industry. As the

company is yet to realize such an achievement in the region, the path towards such fulfillment

has to be strategic and planned. Marketing department will enable differentiation of this role;

since now it is scattered in all the departments and slightly concentrated in the Inspection

Department.

The company needs to be aware of the total market available and its share in it. It must study its

competitors closely and scientifically; and not rely on the data received from the satisfaction tests

carried out with the clients. Only through such an approach can it expand and be the leading

expert.

One of the modern strategies in marketing is Branding. How strong is our name? Will a new oil

company, oblivious of the service industry of our type, consider us among all the others, just

because of our name? Are we easily accessible? A good example of this is social media

presence. Our competitors, such as SGS and Polucon, are active in social media. They advertise

all the time, and have considerable amount of followers. Could we do the same?

6.2. Revenue Generation from Retained Samples.

After being retained for three months, the samples are discarded by a NEMA certified client to

whom we incur expenses. However, we could benefit from this and generate profit instead.

Consider the petroleum laboratory; the retained samples include heavy fuel oils, jet and, mogas,

among others. These are valuable products which could be used to make heavy diesel oil (HDO)

which can be sold to large companies such as the Bamburi Cement Limited for mass heating.

Another option would be to sell the products as they are to those already involved in the

business. Consider that more than 200 half-litre samples are received monthly, making it

about1200 litres per annum!

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6.3. Introduce Ron and Induction Methods

From march 14th

to December 17th

2014, more than 150 samples were received from four

different clients (Intertek Dar-es-salam /ICB Dar-es-salam constituting over 90%) which

required the analysis using RON and Induction method. All the tests were subcontracted to our

competitors, generating revenues for them. We could introduce these methods or let it be

considered in the next fiscal year, so as to retain the earnings for ourselves.

6.4. Quality Control Adjustments.

There are correct procedures for process control. However, there are challenges during their

implementation, especially when a lot of analysis is being carried out when a lot of samples are

received. This makes the daily monitoring of ambient conditions ineffective since it is not carried

out daily as required, and is omitted when there are analyses during the weekend. Because of

this, it will be wise to make it a responsibility of a particular person (as I was during my

internship) to monitor the conditions.

The QC runs for flash points (both Abel and Pertens) should also be done on time to ensure real

time monitoring of the performance of the instruments. I recommend a notice on the bench near

the instrument reminding the analyst on this.

6.5. Position and Working of the Thermometers

The wall thermometer in the petroleum laboratory is placed in close proximity with the water

bath (labeled Copper Conradson test). This might create a humid atmosphere around the

thermometer, especially during the evening, which might lead to wrong results.

The one in the Agriculture Laboratory has been reading 26oC for more than a month. This means

either the temperature is above the requited standard, or the thermometer is no longer sensitive to

temperature changes. Also, the alcohol thermometer in the Petroleum sample store sometimes

reports a high temperature even when the room is freezing. These two thermometers should be

investigated and the matter corrected.

6.6. Corrosion of Expensive Instruments

The petroleum laboratory has seven taps; three permanently closed and only two frequently

used. Some of the instruments such as the Abel Closed Cup (MBA|LAB|EQP|002) and the

Manual Distillation Unit (MBA|LAB|EQP|086) are positioned close to these taps which has led

them to corrode slowly. They should either be positioned far away from the water taps, or the

water taps close to them closed and only the frequently used ones allowed operating. In my

opinion, only two taps are enough; one to supply water for condensers in the water content and

asphaltenes tests, and another for use by analysts.

Most importantly, the affected instruments should be oiled, since rusting, although slow, is

intravenous and could lead to corrosion of the larger part of the instruments.

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6.7. Quality Control on the Balances, And Special Positioning.

The analytical balance should also have their performance monitored. Although even the

standard weights are available, the QC is rarely performed. This process should also be assigned

to one of the analyst.

The analytical balance in the agriculture laboratory should be positioned where the mercury will

be centrally placed to minimize its instability, and this position marked to ensure no future time

loss in trying to stabilize it.

6.8. Provision of full Personal Protective Equipment (PPEs) for the Attachees

Safety is one of the key considerations in the culture of Intertek. To ensure maximum

compliance, the attachees who will be in the company for at least three months are also fully

protected by the potential hazards in the laboratories by providing them with PPE. Currently, the

dust coats are provided, and the goggles are shared. With the current update on the strictness of

compliance to safety rules, it will be hard to share the goggles. Therefore, the attachees should be

provided with them, including the protective shoes. This could be through retaining two pairs of

PPE from the annual replacement of PPE done by the company.

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7.0. REFERENCES

1. American Standards of Testing and Materials, (ASTM) Volumes 1,2,3,4 and 5.

2. Institute of Petroleum, (IP) volumes 1 and 2.

3. Intertek Statements retrieved from: www. Intertek.com/about/mission, on 8/01/2015 at

1117hr.

4. Metrohm Titrino 716, Instructions for Use 8.716.1013

5. Metrohm 794 Basic Titrino, Instructions for Use 8.794.1003

6. Measurements of density using oscillation-type density meter: Calibration, traceability and

Uncertainties. A Forted, et al.

7. Instructions Manual, DMA 4100M, DMA 4500M and DMA 500M. Filmware version V2.21,

Anton Paar- Str 20 A-8054 Graz/Austria

8. X-ray Fluorescence: Energy- dispersive Analysis (EDXRF). Bachia Arezki.

9. Laboratory Information Management System (LIMS), 2014.

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