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Pakistan Council of Scientific &

Indutrial Research

01 Month Internship Report


By:
Sufian Abrar (Student of BE-IE)
Asad Mumtaz (Student of BE-IE)
From IIEE-PCSIR
Sufianabrar2009@hotmail.com
PREFACE

Over the summer of 2009, we were granted the


unique opportunity to be employed by PCSIR
Laborateries as an Internee. Under the supervision
of Electrical and Instrumentation department, we
were lucky enough to undertake 30 days internship
that expanded my horizons and my way of
thinking.

The purpose of this report is to explain what we did and learned


during our internship period with the Pakistan Council of
Scientific & Industrial Research Environmental Program
(PCSIR) in the Division of Applied Physics. The report is also a
requirement for the partial fulfillment of Industrial Electronics
internship program. The report focuses primarily on the
assignments handled, working environment, successes and short
comings that the intern did encounter when handling various
tasks assigned to him by the supervisor.

Because the various parts of the report reflect the intern’s


shortcomings, successes, observations and comments, it would
be imperative that the recommendations are also given.
Therefore the report gives a number of comments and
recommendations on the internship programme.
It is hoped that this report would serve as a
cardinal vehicle to the improvement of the
internship program.

Acknowledgemen
t

The whole praise is to almighty Allah, creator of


this universe. Who made us the super creature
with great knowledge and who able me to
accomplish this work, we feel great pleasure in
expressing my deepest appreciation and heartiest
gratitude to the staff of PCSIR-Karachi for their
guidance and great help during the internship
period.

We would like to express our deepest affection for


our parents and our friends who prayed for our
success and encouraged us during this internship
period.

A token of special thanks to the following people


who had been very friendly, co-operated with us
throughout our internship period in APPLIED
PHYSICS department and made it possible for us to
learn and gather information. These are the people
who in spite of their busy scheduling took time out
to explain to us the procedures and mechanics of
work in the organization.
We would like to express my deepest thanks to
Muhammad and Dr. Yaqoob, who really gave their
best of time to us and we really learned a lot from
them in a very short period.

Introduction

Pakistan Council of Scientific and Industrial Research (PCSIR); was


established in 1953 under Societies Act to promote the cause of Science
and Technology in the country. Since 1973, it is functioning under the
Act of Parliament, which was amended in 1984. Chief Executive of the
Council is the Chairman who is appointed by the Federal Government.
The 21- member Council is the policy making body of the PCSIR, which
is composed of Chairman, three Members of the Governing Body, three
Directors of PCSIR Laboratories, four representatives from four
ministries, four Directors of Industries, one from each province and six
representatives of the industry.
The Governing Body is the executive organ of the Council and
comprises of the Chairman and three full-time members viz Member
(Science), Member (Technology) and
Member (Finance), nominated by the
Government.The Head Office of the PCSIR
is functioning at Islamabad where offices of
the Chairman, Member (Science), Member
(Technology), Member (Finance) and
Secretary PCSIR are located. The Science
Wing is headed by Member (Science), who
supervises matters relating to R&D, Training, International Affairs and
Scientific Information Services. The Technology Wing is headed by the
Member (Technology), who looks after the matters relating to
Technology, Industrial Liaison and Civil Works. The Finance Wing is
headed by the Member (Finance) who is in charge of activities in
Finance and Audit and Accounts Divisions. The Chairman is assisted by
the Secretary and Administration and Establishment Wings, working
directly under him.
There are eleven Laboratories / Units and five HRD Centres established
throughout the country, headed by Director Generals / Directors who
directly report to the Chairman. In Head Office 150 officers / staff
including 07 Directors are working in different divisions / wings. There
are 681 Scientists / Engineers / Technologists working in different
Laboratories out of which 80 are Ph.D.s and others have M.Sc.
/MS/M.Phil. /B.E. degrees in multidisciplinary fields. These
are supported by 1656 technical and skilled staff and 178 administrative
staff.

Pakistan Council of Scientific and Industrial Research


Laboratories Complex Karachi is a multifunctional unit.
The laboratory has highly educated, well trained and
skilled personnel, having expertise in different scientific
fields with broad vision especially in Pharmaceutical,
Marine, Food Sciences, Applied Chemistry, Chemical
Engineering, Physics, Computers, Instrumentation Design
and Development etc.
PCSIR Laboratories Complex, Karachi is a premier R & D
unit of PCSIR, which is committed to produce high quality
research / products by exploiting, indigenous natural
resources for the progress and development of the
country.
PCSIR Laboratories Complex, Karachi has the honors to
be the first multidisciplinary Unit in the whole Ministry of
Science and Technology to obtain the prestigious
international award of being certified to ISO –9001 for the
quality of service, which it provides to industries among
organizations of public and private sectors. Recently
PCSIR Laboratories Complex, Karachi has been
accreditated in ISO 17025 from Pakistan National
Accreditation Council (PNAC), MoST.
ACTIVITIES

The broad-based activities of the PCSIR encompass almost the entire industrial sector
in the country; for the industrial units in operation have their ground-work in science and
technology in which the PCSIR is both prominent and all too visible an organization on
the national plan. The PCSIR being the foremost industrial R & D organization is the
largest producer of indigenous technologies in an organized fashion. The R & D projects
of the PCSIR fall into two major categories:
Those that are sponsored or are user liked.
Those for which a user is likely to be available but has to be found out.
Evaluation of Locally Available Raw Materials
Pakistan is replete with respect to natural resources and their exploitation should have
been the top priority in the process of industrialization of the country but instead of
using local materials, a consumer industry based on imported raw materials was largely
established.

PCSIR's main thrust in the starting years was to investigate the physico-chemical
composition of the locally available raw materials and to find out their possible
utilization. Out of the large number of research publications (over 4000) that PCSIR
produced during the period, 70 percent relates to the evaluation of local materials. The
data thus generated is the single most important contribution of the PCSIR, which no
other organization in the country can claim. It is available in the form of research
papers, technical bulletins, brochures and reports, etc. It covers the areas from minerals,
ores, clays, forest produced herbs, plants to marine and animal wastes. PCSIR can
undertake survey and evaluation studies of raw materials and products on behalf of the
industry.
Process and Product Development
The Scientists and Technologists of PCSIR developed 684 industrial processes and
products and 350 numbers of patents, mostly based on the locally available raw
materials. Out of these nearly 400 processes have commercially been exploited on
industrial scale. It has also executed around 50 Annual Development Programme (ADP)
projects, which were mainly pilot plant studies, based on the data generated on the
laboratory level.
Investigative Analysis and Import substitution
A large number of formulated products are being imported at exorbitant rates resulting
in the expenditure of costly foreign exchange by the textile, leather, pharmaceutical,
cosmetics, household chemicals, food additives and consumer products industries in the
form of emulsions, surfactants, resins, adhesives, plastic parts, perfumes, flavors and
other chemical and non-chemical products. Most of these items are imported under
brand names. The expertise and technical manpower available in the PCSIR have been
able to decode and analyses over 2000 of these products and helped the local SME's in
the development of import-substituted materials.

Analytical and Testing Services


PCSIR is capable of undertaking large number of tests of raw materials and industrial
products and can provide physical, chemical, chromatographic and spectroscopic
analytical services in the diversified fields.

It has the requisite highly qualified, trained and experienced resource manpower not
available which is in any other organisation of the country.

It has the necessary infrastructure in terms of quality control, equipment and analytical
instruments and laboratories.

It has the capability to investigate, improve and introduce latest methodology of testing
and quality control in the production and application.

PCSIR at present is serving over 4000 SME's / clients all over the country annually in
quality control, analytical and testing area.
Quality Control Services to the Exporters
The major exports of Pakistan are textile, leather, food, sports and surgical goods and
products, which are based on locally available raw materials. The exports are essentially
made to western European countries, America and Japan. These countries are becoming
more quality conscious and introducing various parameters and checks to monitor the
quality of the imported products. ISO 9000, 14000 and 17025 etc standards are being
brought in to monitor the desired quality. Pakistan has faced much competition in the
region for exports and in order to remain competitive there is a need to educate, support
and provide technical and quality control services to the producers and exporters of
goods.

PCSIR is doing its best to extend these services to the exporters. Textile and leather
exportable items are examined for forbidden dyes, PCP, formaldehyde, heavy metals,
pesticides and fungicides and most of other undesirable chemicals on the request of the
exporters and issuing analytical reports / certificates which are being accepted in Europe
and elsewhere. PCSIR has developed credibility for these test reports. Similarly food
items being exported by Nestle and others are being tested for their microbial
contamination and shelf life. Exporters of surgical goods, and sports goods are also
getting technical and analytical help from PCSIR. Under the supervision of EPB and
technical guidance of Mineral and Metallurgy Research Centre of PCSIR, a Material
Testing Laboratory has been established at Sialkot to Cater to the needs of the exporters
of that area and PCSIR is imparting training to the technical staff posted in M T Labs
Sialkot.
Services to Government Departments and NGOs
Various Government departments such as Customs, Excise, Police, Administration,
Health and NGO's avail the analytical testing and advisory services of PCSIR in resolving
disputes, fake and genuine products categorization investigative matters, narcotics,
screening of medicines for steroids, etc.

Help in Crisis Situations


Due to the availability of diverse expertise and extensive laboratory infrastructure,
PCSIR enjoy the status of focal point in the crisis situations and its scientific and
technical staff is always ready to extend to the local Administration the technical help to
solve the problems and ameliorate the situation. The major areas where PCSIR has
significant contributions are:
Trouble shooting problems of the industry
Fire accidents
Poisonous gases leakage
Explosions

Environment and Pollution Control


The expertise available in PCSIR in the field of Environment and Pollution Control is not
only training of its own S&T staff in the assessment, monitoring and control systems of
air, water and soil pollution but is also helping the local industry for self-monitoring and
impact assessments. It is also helping the Ministry of Environment, Local Government
and Rural Development, Planning Division, Ministry of Industries in framing and
implementing National Environment Quality Standards (NEQS) of air, water, industrial
liquid and solid effluents and gasses emissions. PCSIR is also assisting the local industry
in acquisition, modification of existing plants, handling of hazardous wastes, treatment of
effluents, control of emissions, etc. for environmentally clean and safe productions.
PCSIR laboratories have already been recommended by the EPA as environmental
laboratories to carry out testing of environment samples. PCSIR scientists/technologists
are helping Ministry of Environment to prepare, organize and execute training
programmes in the field of environment monitoring and assessment.

ISO - 9000/14000 Certification


On the introduction of the ISO-9000 series of the standards, the specified quality of the
products has become a vital issue for all the companies of the country to conduct their
business according to the requirements of applicable standards.

In Pakistan PCSIR is the only organization, which is capable of doing quality


management work successfully as it has all desired facilities available within its premises
in each of the province of the country. PCSIR has over one hundred different types of
latest equipments and highly trained manpower to test and evaluate a factory's raw
materials, in process inventories, finished products and the packed products which are to
be marketed. The manpower of PCSIR is also capable of doing the Environmental Impact
Assessment studies in and around the vicinity, a plant is operating.

The scientists of PCSIR are well aware of the ISO-9000, ISO-14000 and WTO
requirements which have introduced new world order for improving the quality of
products, services and management systems of the organizations. In this context, PCSIR
plan to get ISO-9000 certification and accreditation against ISO-17025. In the very
recently under a joint project of MOST & M/O Commerce. Some 500 industries have
been examined by PCSIR scientists for the certification and about 250 industries have
adopted/received certification for ISO 9000 under the programme. An Incentive grants
of Rs. 200,000/- has also been provided to each successful client upon recommend
actions of PCSIR.

Workshops, Seminars & Training Programmes


PCSIR arranges seminars, workshops and training porogrammes in the specialized fields
for the senior technical staff of the industry in order to update the knowledge of
industrial workers and to teach the modern techniques, skills and latest methods for
improving the quality and standards of their industrial products. Some of the workshops
and training courses held in PCSIR which were well attended and greatly appreciated by
the relevant industry included:
"Cathode Protection Techniques" for solving corrosion problems in the industry.
New Techniques in Metalography.
Technical training on ore beneficiation to the staff working at the Saindak copper ore
project.
129 Technical Managers, Quality Control Managers, Calibration Managers received
training in three batches in the sophisticated field of Metrology and Calibration.
Various training programmes were held in leather processing, leather finishing, and
quality control for the employees of the leather industry.
Workshop on "Essential Oils, perfumes and Flavors" was held for the benefit of
Cosmetics toiletries, flavors, perfumes household chemical manufactures.
Workshop on "food Preservation" was held for the food and beverage industry.
Training programme in "Cereal Technology and mycotoxins" for the RCD countries.
Workshop on "Oilseed Expelling Systems" for the Expeller manufacturers.
Seminar on "Synthetic Dyes and Intermediate Chemicals" for the local dye industry

Pre-Fesibility, Feasibility & Techno-Economic Studies


PCSIR has experienced and trained scientific and technical manpower to undertake these
studies on behalf of the industry. A number of technical reports and pre-feasibility
studies has been executed by PCSIR on the request of the local industry, Government
agencies such as PUNJMIN, RDC, NDFC, SDA, BDA for survey, evaluation, upgrading of
raw materials required and projects based on the locally available raw materials.

Rural Support Technologies


PCSIR has developed a number of technologies for the uplift of the rural areas of the
country including:
Improved and modified village level sugarcane crusher developed under US AID
programme.
Modified Oil Seed Expeller developed under IDRC, Canada funded project.
Development of erucic acid and glucocinolate-free rapeseeds (crucifers) under PL-480
project.
Bench Mark of Sugar Recovery from sugarcane for the farmers, project funded by
MINFAL, Government of Pakistan.
Seed Decorticating Machine.

Nut Cracking Machine - hand operated as well as power operated for Agha Khan rural
support programme.
Potable water technology.
Carpet making machine.
Household disinfectants.
Preservation of vegetables and Fruits Technologies.

Major Fields Developed


The following are some of the major fields of R&D where necessary expertise, trained
and experienced scientific and technical manpower and infrastructure of labs and
equipment has been established which can cater to the needs of the local industry.
Applied Chemistry / Industrial Chemistry
Pharmaceutical and fine chemicals
Textile Dyes and Pigments
Textile, Sugar and Paper Chemicals
Polymers and Plastics
Cosmetics and Household Chemicals
From Plants and Herbs
Industrial Essential Oils
Oils, Fats, Soaps and Detergents
Leather Chemicals
Medicinal Water Conditioning
Pesticides and Insecticides
Inorganic and Industrial Chemicals
Phytochemicals
Narcotic Testing Kits
Medical Diagnostic Kits
Fillers for Rubber and Plastic Products
Petroleum Products

Biotechnology, Food Technology and Fermentation


Preservation of Food Materials especially through Dehydration of Vegetables and
Fruits
Synthetic beverage concentrates
Vinegar from molasses, apples, dates, etc.
Commercial food sauces
Bating agent for tanneries
Mushroom production.
Fortified breads
Meat and meat products.
Ice cream mixes.
Pickles, jams, jellies and sweets.
Baby foods, low calorie and high energy food supplements
Milk and milk products
Food additives and preservatives
Microbial enzymes
Animal and poultry formulated feeds
Soya bean meat and related products

Minerals and Metallurgy


Mineralogy and geochemistry
Mineral processing / ore beneficiation.
Pyrometallurgy
Hydrometallurgy
Electrometallurgy
Physical metallurgy
Foundry technology
Corrosion and protection
Development of brighteners and electroplating chemicals
Heat treatment salt compositions
Evaluation of foundry sands moldings, silicates, bentonites and bonded sands
Graphite crucibles
Minerals based chemicals

Glass and Ceramics


Utilization of industrial minerals
Development of all types of Alumino-silicate, magnesite, chrome, chrome-magnesite
and fire clay insulating refractories and evaluation of their raw materials.
Soda-lime silica glass products such as container glasses, signal glasses and dome
glasses.
Rapid hardening cements
Beneficiation of glass sands
Acid proof cement tiles and bricks
Frits and enamels including acid resistant
Low temperature and high temperature glazes for earthenware, stoneware and
porcelain
Pyrometric cones
Grinding wheals, rubbing bricks and horning sticks
High quality glass sands
Ceramic clays
High rupture capacity (HRC) fuses

Applied Biology & Marine Resources


Aflatoxins and mycotoxins in edible materials
Nematode-free nursery and nematicides from natural sources
Biofertilizers from marine sources
Fish culture technology
Biopesticides and insecticides
Preservation of fish, shrimps, etc.,
Marinated, fermented and spiced products from fish, shrimps and shellfish
Fish protein concentrate
Micro-nutrient frits
Fuel and Energy
Smokeless coal briquettes
Biogas generation from animal and agriculture wastes
Carbonization of coals and related materials
Easily ignitable briquettes
Humic acids from coal
Gel fuels
Smokeless stove technology

Applied Physics and Instrumentation


Design and development of laboratory instruments:
pH meters, electrophoresis apparatus deioniser units, temperature and humidity
controllers, water baths, hot-plate magnetic stirrers, ovens, heating mantles, rotary
evaporators, melting point apparatus, crucible and muffle furnaces, orbital shaker.
Technical assistance for product development and design optimization of electrical
goods.
Test and performance evaluation of electrical goods for standardization.
Training of industrial technical manpower.
Repair and maintenance of laboratory equipment.

Leather Technology
Bacterial bating agents.
Industrial leather processing technology.
Processes for garment leather, shoe upper, sole leather, etc.
Leather auxiliaries and chemicals.

Environment & Pollution Control


Industrial effluents.
Air, water and land pollution control measures.
Wastes characterization and treatments.
Monitoring methodologies on air, water, soil and hazardous wastes.
Environmental management and auditing.
Environment impact assessment and environment impact statements.
Laboratory back up for the assessment of emissions and particulate matter

Solar Technology
Development of equipment and appliances based on solar energy such as solar water
heaters, solar space heating and cooling, solar stills for desalination of saline waters,
solar photovoltaic systems. xi. Rural Development Technologies
Improved sugarcane crusher.
Improved and modified oil expeller.
Carpet making machine.
Nut cracking machine.
Decorticating machine for oils seeds.
Rice bran utilization
Water conditioning for drinking.
Fruit drying and preservation

Standards and Metrology


Maintaining primary, secondary & working standards of based & derived quantities
including linear, dimensional and angle measurements, surface measurements, mass,
volumes, density measurements, electricity, time, frequency, magnetism pyrometry,
temperature, pressure, hardness, refractive index, pH and conductivity measurements.

Calibration of industrial and laboratories equipments.

Engineering
Design and development of precision machines and machine tools, jigs, moulds, dies and
spare parts of high precision.

Production of components of satellites.

Machining, drilling, and sizing machine components on CNC machine. Designing and
fabrication of pilot plants, reaction vessels, shakers, vacuum dryers, filtration equipment,
etc.
Training
We received no formal training as such in terms of
our individual project. It was our responsibility to
become familiar with the system and the
development platform.

However, in this internship program, we learned


‘team building’ exercises. Here we studied how
different ‘types’ of people in the workplace
interacted. For example, we discovered firsthand
how our ‘type’ (Creator-Innovator) clashed with the
‘Thuster-Organiser’ type and how to organize types
of people to build an effective and balanced team.

In the following session we are discussing what


type of process involved in our internship.
Electrical House
wiring
Normally in Pakistan, there is mainly one condition
followed which provide about 220 volts alternating
current(AC) in home faculty of about 50 hertz frequency
and the colour coding of hot and cold wires are red and
black. Red wire gives the way of phase and black wire
gives neutral. We are advised not to connect cold wire to
switch because when hot wire connect direct to the load
theres a cause of low power provide to the load when the
switch is off, for this reason we have to connect always
hot wire for switching purpose and cold wire directly
connected to the load.
Modern outlets have three different shaped holes to
assure plugs can only be inserted in one way. Two of the
holes are considered grounds, for reasons of safety.
Proper grounding and the use of fuses are important to
maintain electrical safety in the home.

Home wiring

Typically, homes in Paksitan receive 220 volts of AC


electricity. Certain high-power devices, such as an
electric stove, use the full 220 volts. The rest of the
outlets in the house use 110 volts.

Wires into home

Usually, three copper wires come into the home. Two are
covered in black insulation and one has white insulation.
Sometimes one wire is red instead of black. Each black or
red wire is called a "hot" wire and has 110-volt AC. The
white wire is called the "common" and is grounded at the
power station.Measuring across the two hot wires results
in 220 volts. Measuring the voltage between a black (or
red) and white wire, results in 110-volt AC.

Wiring configuration

Copper wire

Copper wire is used because it is a good conductor of


electricity. Materials that do not conduct electricity as
good usually have a higher resistance. This results in
wasted energy and the tendency to get hot, which could
be a safety hazard.

In the 1960s many electrical contractors started to use


aluminum wire instead of copper. Aluminum is almost as
good of a conductor as copper, but it is much less
expensive. After a number of years, it was found that this
type of wiring caused a potential fire hazard. Problems
due to expansion caused overheating at connections
between the wire and switches, outlets, or splices. Many
homes had to be re-wired, although there still are many
that still have aluminum wiring but have never had
problems.

Wall outlets

The wall outlets usually have a one wide slot, one narrow
slot and one round-with-flat-bottom hole. This is to
assure that each part of the plug will be used as it is
supposed to and to increase safety. Older outlets have
both slots the same size and no round hole.

Typical wall outlet

Outlet slots

The narrow slot is considered "hot" and is where the


alternating current power comes out. The wiring behind
the outlet to this slot is usually black in the Pakistan. The
wide slot is considered the "common" and is supposed to
be grounded. Using the white wire as a common
grounded wire, means that everyone is working from the
same zero voltage position.
Round hole

The hole that is round on the top and flat on the bottom
is an extra ground. Usually the wire behind the wall
outlet has green insulation. Sometimes it is a bare wire.
This extra ground is to make sure your utensils are
properly grounded in the situation that someone had
improperly wired the house. It is an extra safety
measure.

Common wire

Although the white wire is not supposed to be a "hot"


wire, in some cases it is used that way, especially in older
homes that have the old style outlets. In general, this is
acceptable, but it can result in problems. If you touch a
common wire that is properly grounded, you should not
get a shock. But if that wiring has made it hot, you can
get a shock. Also, by using the white wire where the
black should be used, you may cause a short circuit.

Safety

Proper grounding and the use of fuses are important for


protection against shock, as well as to prevent electrical
overheating and fire hazards

Grounding

Correct grounding is very important. Often ground wires


are connected to water pipes that normally go into the
ground. Connecting to a hot water pipe means that the
water heater is between the connection and the ground.
The water heater may have plastic parts that would
insulate the connection to ground. Thus, using a hot
water pipe is not a good idea.

Another consideration in using water pipes to ground the


circuit is that plastic piping is often being used in
plumbing. You must make sure there are no plastic pipes
between your connection and the outside earth or
ground.

Fuses

Fuses and circuit breakers are used as a safety measure


in case of short circuits. A fuse or circuit breaker will
break the connection if more current is passing through
the wire than is considered safe. This will prevent the
house wiring to overheat and start a fire.

Most homes now use circuit breakers instead of fuses.


One reason is because people with bad wiring in their
homes that constantly blow out fuses, would then force
pennies in the fuse receptacles, thus bypassing the
requirement for a fuse. This removed the aggravation, as
well as the expense of buying new fuses, but it also often
resulted in serious electrical fires in the house.

Summary

Most homes use both 220- and 110-volt AC electricity.


Wires have black, red, white or green insulation,
depending on their use. The holes in modern outlets
assure plugs can only be inserted in one way. Proper
grounding and the use of fuses are important to maintain
electrical safety in the home.
Contactor
In semiconductor testing, contactor can also refer to the specialised
socket that connects the device under test.

In process industries a contactor is a vessel where two streams


interact, for example, air and liquid.
A contactor is an electrically controlled switch used for switching a
power circuit, similar to relayexcept with higher amperage
ratings. [1] A contactor is controlled by a circuit which has a much
lower power level than the switched circuit. Contactors come in
many forms with varying capacities and features. Unlike a circuit
breaker, a contactor is not intended to interrupt a short
circuit current.

Contactors range from those having a breaking current of several


amps and 24 V DC to thousands of amps and many kilovolts. The
physical size of contactors ranges from a device small enough to
pick up with one hand, to large devices approximately a meter
(yard) on a side.
Contactors are used to control electric
motors, lighting, heating, capacitor banks, and other electrical
loads.
Construction
A contactor is composed of three different items. The contacts are the
current carrying part of the contactor. This includes power contacts,
auxiliary contacts, and contact springs. The electromagnet provides the
driving force to close the contacts. The enclosure is a frame housing the
contact and the electromagnet. Enclosures are made of insulating materials
likeBakelite, Nylon 6, and thermosetting plastics to protect and insulate the
contacts and to provide some measure of protection against personnel
touching the contacts. Open-frame contactors may have a further
enclosure to protect against dust, oil, explosion hazards and weather.
High voltage contactors (greater than 1000 volts) may use vacuum or an
inert gas around the contacts.
Magnetic blowouts use blowout coils to lengthen and move the electric arc.
These are especially useful in DC power circuits. AC arcs have periods of
low current, during which the arc can be extinguished with relative ease,
but DC arcs have continuous high current, so blowing them out requires the
arc to be stretched further than an AC arc of the same current. The
magnetic blowouts in the pictured Albright contactor (which is designed for
DC currents) more than double the current it can break, increasing it from
600 A to 1,500 A.
Sometimes an economizer circuit is also installed to reduce the power
required to keep a contactor closed; an auxiliary contact reduces coil
current after the contactor closes. A somewhat greater amount of power is
required to initially close a contactor than is required to keep it closed. Such
a circuit can save a substantial amount of power and allow the energized
coil to stay cooler. Economizer circuits are nearly always applied on direct-
current contactor coils and on large alternating current contactor coils.
A basic contactor will have a coil input (which may be driven by either an
AC or DC supply depending on the contactor design). The coil may be
energized at the same voltage as the motor, or may be separately
controlled with a lower coil voltage better suited to control byprogrammable
controllers and lower-voltage pilot devices. Certain contactors have series
coils connected in the motor circuit; these are used, for example, for
automatic acceleration control, where the next stage of resistance is not cut
out until the motor current has dropped
Operating Principle
Unlike general-purpose relays, contactors are designed to be directly
connected to high-current load devices. Relays tend to be of lower capacity
and are usually designed for both normally closed and normally
open applications. Devices switching more than 15 amperes or in circuits
rated more than a few kilowatts are usually called contactors. Apart from
optional auxiliary low current contacts, contactors are almost exclusively
fitted with normally open contacts. Unlike relays, contactors are designed
with features to control and suppress the arc produced when interrupting
heavy motor currents.
When current passes through the electromagnet, a magnetic field is
produced; which attracts the moving core of the contactor. The
electromagnet coil draws more current initially, until
its inductance increases when the metal core enters the coil. The moving
contact is propelled by the moving core; the force developed by the
electromagnet holds the moving and fixed contacts together. When the
contactor coil is de-energized, gravity or a spring returns the electromagnet
core to its initial position and opens the contacts.
For contactors energized with alternating current, a small part of the core is
surrounded with a shading coil, which slightly delays the magnetic flux in
the core. The effect is to average out the alternating pull of the magnetic
field and so prevent the core from buzzing at twice line frequency.
Most motor control contactors at low voltages (600 volts and less) are air
break contactors; i.e., ordinary air surrounds the contacts and extinguishes
the arc when interrupting the circuit. Modern medium-voltage motor
controllers use vacuum contactors.
Motor controlled contactors can be fitted with short-circuit protection (fuses
or circuit breakers), disconnecting means, overload relays and an
enclosure to make a combination starter.
Ratings

Contactors are rated by designed load current per contact (pole), maximum
fault withstand current, duty cycle, voltage, and coil voltage. A general
purpose motor control contactor may be suitable for heavy starting duty on
large motors; so-called "definite purpose" contactors are carefully adapted
to such applications as air-conditioning compressor motor starting. North
American and European ratings for contactors follow different philosophies,
with North American general purpose machine tool contactors generally
emphasizing simplicity of application while definite purpose and European
rating philosophy emphasizes design for the intended life cycle of the
application.
Current rating of the contactor depends on utilization category. For
example IEC Categories are described as:

 AC1 - Non-inductive or slightly inductive rows


 AC2 - Starting of slip-ring motors
 AC3 - Starting of squirrel-cage motors and switching off only after the
motor is up to speed. (Make Locked Rotor Amps (LRA), Break Full
Load Amps (FLA))
 AC4 - Starting of squirrel-cage motors with inching and plugging duty.
Rapid Start/Stop. (Make and Break LRA)
 AC11 - Auxiliary (control) circuits

Applicaions

Lighting control
Contactors are often used to provide central control of large lighting
installations, such as an office building or retail building. To reduce power
consumption in the contactor coils, latching contactors are used, which
have two operating coils. One coil, momentarily energized, closes the
power circuit contacts, which are then mechanically held closed; the
second coil opens the contacts.

Magnetic starter
A magnetic starter is a contactor designed to provide power to
electric motors. The magnetic starter has an overload relay,
which will open the control voltage to the starter coil if it detects
an overload on a motor. Overload relays may rely on heat
produced by the motor current to operate a bimetal contact or
release a contact held closed by a low-melting-point alloy. The
overload relay opens a set of contacts that arewired in series
with the supply to the contactor feeding the motor. The
characteristics of the heaters can be matched to the motor so
that the motor is protected against overload. Recently,
microprocessor-controlled motor protection relays offer more
comprehensive protection of motors.
Perhaps the most common industrial use for contactors is
the control of electric motors.
Induction Motor
The AC induction motor is a rotating electric machine designed to
operate from a three-phase source of alternating voltage. The
stator is a classic three phase stator with the winding displaced
by 120°. The most common type of induction motor has a squirrel
cage rotor in which aluminum conductors or bars are shorted
together at both ends of the rotor by cast aluminum end rings.
When three currents flow through the three symmetrically placed
windings, a sinusoidally distributed air gap flux generating the
rotor current is produced. The interaction of the sinusoidally
distributed air gap flux and induced rotor currents produces a
torque on the rotor. The mechanical angular velocity of the rotor
is lower than the angular velocity of the flux wave by so called
slip velocity.
In adjustable speed applications, AC motors are powered by
inverters. The inverter converts DC power to AC power at the
required frequency and amplitude. The inverter consists of three
half-bridge units where the upper and lower switch is controlled
complimentarily. As the power device's turn-off time is longer
than its turn-on time, some dead-time must be inserted between
the turn-off of one transistor of the half-bridge and turn-on of it's
complementary device. The output voltage is mostly created by a
pulse width modulation (PWM) technique. The 3-phase voltage
waves are shifted 120° to each other and thus a 3-phase motor
can be supplied.

Methods of Starting Induction Motor


As we know, once a supply is connected to a three phase
induction motor a rotating magnetic field will be set up in the
stator, this will link and cut the rotor bars which in turn will induce
rotor currents and create a rotor field which will interact with the
stator field and produce rotation. Of course this means that the
three phase induction motor is entirely capable of self starting.
The need for a starter therefore is not, conversely enough, to
provide starting but to reduce heavy starting currents and provide
overload and no-voltage protection.
There are a number of different types of starter including ‘The
Direct On-line Starter’, ‘The Star- Delta Starter’, ‘and Auto-
Transformer ’and‘Rotor resistance’.

Direct-on-Line Starter (DOL)


The DOL starter switches the supply directly on to the contacts of
the motor.
As the starting current of an induction motor can be 6-8 times the
running current the DOL starter is typically only used for motors
with a rating of less than 5kW.

Star Delta starter


This is the most common form of starter used for three phase
induction motors. It achieves an effective reduction of starting
current by initially connecting the stator windings in star
configuration which effectively places any two phases in series
across the supply. Starting in star not only has the effect of
reducing the motor’s start current but also the starting torque.
Once up to a particular running speed a double throw switch
changes the winding arrangements from star to delta whereupon
full running torque is achieved.
Such an arrangement means that the ends of all stator windings
must be brought to terminations outside the casing of the motor.

Auto-Transformer Starting
This method of starting reduces the start current by reducing the
voltage at start up. It can give lower start up currents than star-
delta arrangements but with an associated loss of torque. It is not
as commonly utilized as other starting methods but does have the
advantage that only three connection conductors are required
between starter and motor.

Rotor Resistance Starter


If it is necessary to start a three phase induction motor on load
then a wound rotor machine will normally be selected. Such a
machine allows an external resistance to be connected to the
rotor of the machine through slip rings and brushes. At start-up
the rotor resistance is set at maximum but is reduced as speed
inceases until eventually it is reduced to zero and the machine
runs as if it is a cage rotor machine

Synchronous motor
A synchronous electric motor is an AC motor distinguished by
a rotor spinning with coils passing magnets at the same rate as
thealternating current and resulting magnetic field which drives it. Another
way of saying this is that it has zero slip under usual operating conditions.
Contrast this with an induction motor, which must slip in order to
produce torque. They operate synchronously with line frequency. As with
squirrel-cage induction motors; speed is determined by the number of pairs
of poles and the line frequency. Synchronous motors are available in sub-
fractional self-excited sizes to high-horsepower direct-current
excited industrial sizes. In the fractional horsepower range, most
synchronous motors are used where precise constant speed is required. In
high-horsepower industrial sizes, the synchronous motor provides two
important functions. First, it is a highly efficient means of converting ac
energy to work. Second, it can operate at leading or unity power factor and
thereby provide power-factor correction.
There are two major types of synchronous motors: non-excited and direct-
current excited.
Non-excited motors are manufactured
in reluctance and hysteresis designs, these motors employ a self-starting
circuit and require no external excitation supply.
Reluctance designs have ratings that range from sub-fractional to about
30 hp. Sub-fractional horsepower motors have low torque, and are
generally used for instrumentation applications. Moderate torque, integral
horsepower motors use squirrel- cage construction with toothed rotors.
When used with an adjustable frequency power supply, all motors in the
drive system can be controlled at exactly the same speed. The power
supply frequency determines motor operating speed.
Hysteresis motors are manufactured in sub-fractional horsepower ratings,
primarily as servomotors and timing motors. More expensive than the
reluctance type, hysteresis motors are used where precise constant speed
is required.
DC-excited motors — made in sizes larger than 1 hp, these motors require
direct current supplied through slip rings for excitation. The direct current
can be supplied from a separate source or from a dc generator directly
connected to the motor shaft
Slip rings and brushes are used to conduct current to the rotor. The rotor
poles connect to each other and move at the same speed - hence the
name synchronous motor.
Synchronous motors fall under the category of synchronous machines
which also includes the alternator (synchronous generator). These
machines are commonly used in analog electric clocks, timers and other
devices where correct time is required.
The speed of a synchronous motor is determined by the following formula:

Where v is the speed of the rotor (in rpm), f is the frequency of the AC
supply (in Hz) and n is the number of magnetic poles.
Parts
 A synchronous motor is composed of the following parts:
 The stator is the outer shell of the motor, which carries the armature
winding. This winding is spatially distributed for poly-phase AC
current. This armature creates a rotating magnetic field inside the
motor.
 The rotor is the rotating portion of the motor. It carries field winding,
which may be supplied by a DC source. On excitation, this field
winding behaves as a permanent magnet.
 The slip rings in the rotor, to supply the DC to the field winding, in the
case of DC excited types

Operation
The operation of a synchronous motor is simple to imagine. The armature
winding, when excited by a poly-phase (usually 3-phase) winding, creates a
rotating magnetic field inside the motor. The field winding, which acts as a
permanent magnet, simply locks in with the rotating magnetic field and
rotates along with it. During operation, as the field locks in with the rotating
magnetic field, the motor is said to be in synchronization.
Once the motor is in operation, the speed of the motor is dependent only
on the supply frequency. When the motor load is increased beyond the
break down load, the motor falls out of synchronization i.e., the applied load
is large enough to pull out the field winding from following the rotating
magnetic field. The motor immediately stalls after it falls out of
synchronization.
Starting methods
Synchronous motors are not self-starting motors. This property is due to
the inertia of the rotor. When the power supply is switched on, the armature
winding and field windings are excited. Instantaneously, the armature
winding creates a rotating magnetic field, which revolves at the designated
motor speed. The rotor, due to inertia, will not follow the revolving magnetic
field. In practice, the rotor should be rotated by some other means near to
the motor's synchronous speed to overcome the inertia. Once the rotor
nears the synchronous speed, the field winding is excited, and the motor
pulls into synchronization.
The following techniques are employed to start a synchronous motor:

 A separate motor (called pony motor) is used to drive the rotor


before it locks in into synchronization.
 The field winding is shunted or induction motor like arrangements
are made so that the synchronous motor starts as an induction
motor and locks in to synchronization once it reaches speeds near
its synchronous speed.

 Reducing the input electrical frequency to get the motor starting


slowly, Variable-frequency drives can be used here which
haveRectifier-Inverter circuits or a Cycloconverter circuits.

Special properties
Synchronous motors show some interesting properties, which find
applications in power factor correction. The synchronous motor can be run
at lagging, unity or leading power factor. The control is with the field
excitation, as described below:

 When the field excitation voltage is decreased, the motor runs in


lagging power factor. The power factor by which the motor lags varies
directly with the drop in excitation voltage. This condition is called under-
excitation.

 When the field excitation voltage is made equal to the rated voltage,
the motor runs at unity power factor.
 When the field excitation voltage is increased above the rated
voltage, the motor runs at leading power factor. And the power factor
by which the motor leads varies directly with the increase in field
excitation voltage. This condition is called over-excitation.
 The most basic property of sycho motor is that it can be use as a
CAPACITOR OR INDUCTOR both. Hence in turn it improves the
power factor of system.

The leading power factor operation of synchronous motor finds application


in power factor correction. Normally, all the loads connected to the power
supply grid run in lagging power factor, which increases reactive power
consumption in the grid, thus contributing to additional losses. In such
cases, a synchronous motor with no load is connected to the grid and is run
over-excited, so that the leading power factor created by synchronous
motor compensates the existing lagging power factor in the grid and the
overall power factor is brought close to 1 (unity power factor). If unity power
factor is maintained in a grid, reactive power losses diminish to zero,
increasing the efficiency of the grid. This operation of synchronous motor in
over-excited mode to correct the power factor is sometimes called
as Synchronous condenser.
Uses

 Synchronous motors find applications in all industrial applications


where constant speed is necessary.
 Improving the power factor as Synchronous condensers.
 Electrical power plants almost always use synchronous generators
because it is important to keep the frequency constant at which the
generator is connected.
 Low power applications include positioning machines, where high
precision is required, and robot actuators.
 Mains synchronous motors are used for electric clocks.
 Record player turntables

Advantages
Synchronous motors have the following advantages over non-synchronous
motors:

 Speed is independent of the load, provided an adequate field current


is applied.
 Accurate control in speed and position using open loop controls,
eg. Stepper motors.
 They will hold their position when a DC current is applied to both the
stator and the rotor windings.
 Their power factor can be adjusted to unity by using a proper field
current relative to the load. Also, a "capacitive" power factor, (current
phase leads voltage phase), can be obtained by increasing this
current slightly, which can help achieve a better power factor
correction for the whole installation.
 Their construction allows for increased electrical efficiency when a
low speed is required (as in ball mills and similar apparatus).
 They run either at the synchronous speed else no speed is there.

X-Ray Diffraction
In PCSIR, XRD is of Siemens brand and PCSIR have only
two Xrd machines in which one is functioning and other is
malfunctioned.
X-ray crystallography
X-ray crystallography is a method of determining the arrangement
of atoms within a crystal, in which a beam of X-rays strikes a crystal
and diffracts into many specific directions. From the angles and intensities
of these diffracted beams, a crystallographer can produce a three-
dimensional picture of the density of electrons within the crystal. From this
electron density, the mean positions of the atoms in the crystal can be
determined, as well as their chemical bonds, their disorder and various
other information.
Since many materials can form crystals — such
as salts, metals, minerals, semiconductors, as well as various inorganic,
organic and biological molecules — X-ray crystallography has been
fundamental in the development of many scientific fields. In its first decades
of use, this method determined the size of atoms, the lengths and types of
chemical bonds, and the atomic-scale differences among various materials,
especially minerals and alloys. The method also revealed the structure and
functioning of many biological molecules, including vitamins, drugs,
proteins and nucleic acids such as DNA. X-ray crystallography is still the
chief method for characterizing the atomic structure of new materials and in
discerning materials that appear similar by otherexperiments. X-ray crystal
structures can also account for unusual electronic or elastic properties of a
material, shed light on chemical interactions and processes, or serve as the
basis fordesigning pharmaceuticals against diseases.
In an X-ray diffraction measurement, a crystal is mounted on
a goniometer and gradually rotated while being bombarded with X-rays,
producing a diffraction pattern of regularly spaced spots known
as reflections. The two-dimensional images taken at different rotations are
converted into a three-dimensional model of the density of electrons within
the crystal using the mathematical method of Fourier transforms, combined
with chemical data known for the sample. Poor resolution (fuzziness) or
even errors may result if the crystals are too small, or not uniform enough
in their internal makeup.
X-ray crystallography is related to several other methods for determining
atomic structures. Similar diffraction patterns can be produced by scattering
electrons or neutrons, which are likewise interpreted as a Fourier
transform. If single crystals of sufficient size cannot be obtained, various
other X-ray methods can be applied to obtain less detailed information;
such methods include fiber diffraction, powder diffraction andsmall-angle X-
ray scattering (SAXS). In all these methods, the scattering is elastic; the
scattered X-rays have the same wavelength as the incoming X-ray. By
contrast, inelastic X-ray scattering methods are useful in studying
excitations of the sample, rather than the distribution of its atoms.

Instructions for Siemens D5000 Diffraktometer (XRD)


Instrument

The software for computing data is the Siemens Diffrac AT


program V3.10. The X-ray tube has a lateral outlet window in the
D5000 diffraktometer. This X-ray tube with earthed anode is
supplied by a kristalloflex 710 X-ray generator which is installed in
console-type housing. An FK 60-04 air insulated X-ray diffraction
tube with Cu anode is suitable for the majority of the diffraction
examinations. The Siemens has a complicated energy dispersifive
(EDX), state of the class for certification. Students will be given
beam time for mineralogy class.

2. Place prepared short microscope slide with clay treatment in


the 1-7/8” square holder and record the sample
identification. If you are using the thick 1-7/8” square glass
slides, record the sample identification.

3. Open XRD door and place slide onto round flexible stub, release
the stub lever and push the slide up until it is tight against the top
of the three fixed feet.

4. Using the “START”, program either Siemens DIFFRACplus -


D5000 #1 (common) or XRD (common), then go to Job
Measurement. A table screen with information for the slide
to be run will appear with a menu bar across the top. The
DQL file can be edited within this section or under the
separate heading of XRD (common) or Siemens DIFFRACplus
- D5000 #1 (common) - Edit DQL. The DQL information
below is standard for most slides.

Scan distance 2o - 34o 2θ

Step size 0.02o (don’t change this)

Step time 0.3 seconds

Scanning rate continuous*


Detector 1

Run time 8 mn 0 s (this will be


calculated from above scan
entries automatically)
*continuous vs step scan - continuous takes 0.3 second to
scan to each 0.02o, where step moves 0.02o every 0.3
second (jumps from one 0.02o to the next).

5. Once the program is set there is not a reason to change unless


the scan distance or step time can improve the pattern or
save beam time. Changes will decrease or increase the run
time for the pattern but could make the diffractogram not
contain an abundance of noise and messy patterns. Edit the
set-up if potassium slides are being run to read, 2o - 15o 2θ.

6. Type in information as needed for each of the headings. The


cursor will be at Raw File. At the prompt type A:\ no more
than 8 characters for file-name or D:\file-name for zip drive.
Use file-names for samples that denote the treatment as well
as sample identification. Example: AF, MgSanta; AF,
MggSanta; AF, KSanta; AF, KHSanta. Move cursor to Sample
Identification. Type the same sample information that is
under Raw File. This will be the heading for your printed
diffractogram output later. Example: Mg-sat., Santa A
horizon. Click cursor to Parameter File, click on Browse,
find Anita and open that DQL file. If you want to edit this file
for scan distance or step time, go to the top menu under
Option, and then edit DQL-file. Click Execute Job, if
everything has been entered correctly. Check the input lines
below table entry box to make sure your file drive is correct
and the file-name is correctly spelled. Once the job is
executed DO NOT stop or abort the run --- the XRD will go
into cardiac arrest.

6. To watch the display for the sample running, go to START,


program Siemens DIFFRACplus – D5000 #1 (common) or
XRD (common), Status Display and click there is the
sample pattern as it is running.
7. To view pattern, go to, START, program Siemens DIFFRACplus - D5000 #1
(common) or XRD (common), then EVA. Select File and open raw XRD
file-name you want to view. If the toolbox is not visible on the screen, click
on the little hammer icon to get the toolbox. The tool box contains all the
options for changes in the patterns display. Click on Background and
replace. Click on Aberrant to remove the extraneous or erogenous peaks
present, then click replace. The option for Smoothing is not desirable for the
XRD diffractogram patterns because the appearance of the XRD will be lost.
The upper visual graph of XRD pattern should be checked closely to make
sure that all the peaks show. The cursor arrow can extend the line above the
peaks so they will be visible when printing. The peak search is under the
toolbox. The peaks can be marked and labeled, if needed.
8. To print a hard copy of the XRD pattern, go to File, then page
& printer set-up. Landscape prints are better for the full
spectrum XRD. The usual set-up options are available for
printing. If title or other changes in actual XRD diffractogram
need to be made, then go to View, then Custom Style. The
screen box will allow for editing title, changing size, font, etc.
The tick marks for the X and Y can be edited or changed. Go
to Print Preview to view the XRD pattern before printing.
Step 7 and 8 can be done while the XRD is running.
Remember to keep the beam busy, so plan your computer
work to be efficient with sample running.

9. Remove the slide from the X-ray holder, place new slide in
holder, record identification, and follow operational steps as
outlined above.

10. A hard copy of the multiple patterns or sequences or


treatments on one page is useful for reports. A color print
can be made or a B/W print with labels for the individual
treatments in power point after the files have been imported
into Excel. The conversion of raw XRD files to the UXD
format will let the data file exchange of XRD files into Excel.
To convert the raw XRD files, go to, START, program
Siemens DIFFRACplus - D5000 #1 (common), then Data File
Exchange. Click on File, and then go to UXD format.
Check the following properties for the conversion of data;
angle & intensity, angle & intensity, column 10 per line 1,
and check the box for skipping headers.

11. Go to File again, open and find the raw XRD file you want to
convert, open the file needed, click on the UXD icon on menu
bar to make the conversion of file, save file to same disk or
place the raw file is stored. If the raw file and UXD file are on
the same disk it will be easier to find and manipulate for
importing to Excel. It is not possible to convert the EVA files
with background, etc. subtracted to a UXD format. EVA
software does not support the transfer of their data to
another program. Of course, they want you to use their
software package; however, it is very difficult to do the
multiple patterns in EVA. The raw files will not have
background, etc. subtracted.

12. Open Excel and open the files from disk with stored UXD data.
Use fixed width and follow the “next” commands. Highlight the
columns of data, go to insert chart as a new sheet, select XY
scatter plot, and follow Excel steps for making a chart and adding
headings/titles, no grids. Highlight the line of the graph and
double click, change line to 2 point size, black or color and no
points (marks). Excel graphs can be copied and transferred to
power point, stacked by making an axis and importing only the
graph lines that need to be stacked, changed to color or left black
and white and labeled with text draw for appropriate axis and
headings.
Contributions to Chemistry and Material science
X-ray crystallography has led to a better understanding of chemical
bonds and non-covalent interactions. The initial studies revealed the typical
radii of atoms, and confirmed many theoretical models of chemical
bonding, such as the tetrahedral bonding of carbon in the diamond
structure, the octahedral bonding of metals observed in ammonium
hexachloroplatinate (IV), and the resonance observed in the planar
carbonate group[ and in aromatic molecules. Kathleen Lonsdale's 1928
structure of hexamethylbenzene established the hexagonal symmetry
of benzene and showed a clear difference in bond length between the
aliphatic C–C bonds and aromatic C–C bonds; this finding led to the idea
of resonance between chemical bonds, which had profound consequences
for the development of chemistry. Her conclusions were anticipated
by William Henry Bragg, who published models of naphthalene and
anthracene in 1921 based on other molecules, an early form of molecular
replacement.
Also in the 1920s, Victor Moritz Goldschmidt and later Linus
Pauling developed rules for eliminating chemically unlikely structures and
for determining the relative sizes of atoms. These rules led to the structure
of brookite (1928) and an understanding of the relative stability of
therutile, brookite and anatase forms of titanium dioxide.
The distance between two bonded atoms is a sensitive measure of the
bond strength and its bond order; thus, X-ray crystallographic studies have
led to the discovery of even more exotic types of bonding in inorganic
chemistry, such as metal-metal double bonds, metal-metal quadruple
bonds, and three-center, two-electron bonds. X-ray crystallography — or,
strictly speaking, an inelasticCompton scattering experiment — has also
provided evidence for the partly covalent character of hydrogen bonds. In
the field oforganometallic chemistry, the X-ray structure
of ferrocene initiated scientific studies of sandwich compounds, while that
of Zeise's saltstimulated research into "back bonding" and metal-pi
complexes. Finally, X-ray crystallography had a pioneering role in the
development of supramolecular chemistry, particularly in clarifying the
structures of the crown ethers and the principles of host-guest chemistry.
In material sciences, many
complicated inorganic and organometallic systems have been analyzed
using single-crystal methods, such asfullerenes, metalloporphyrins, and
other complicated compounds. Single-crystal diffraction is also used in
the pharmaceutical industry, due to recent problems with polymorphs. The
major factors affecting the quality of single-crystal structures are the
crystal's size and regularity;recrystallization is a commonly used technique
to improve these factors in small-molecule crystals. The Cambridge
Structural Databasecontains over 500,000 structures; over 99% of these
structures were determined by X-ray diffraction.

X-ray Diffractometer
X-ray Fluorescence
In Pcsir, there is only one XRF of Bruker company (Siemens
brand) which is so expensive more important equipment for
testing composition.

X-ray fluorescence (XRF) is the emission of characteristic "secondary" (or


fluorescent) X-rays from a material that has been excited by bombarding
with high-energy X-rays or gamma rays. The phenomenon is widely used
forelemental analysis and chemical analysis, particularly in the investigation
ofmetals, glass, ceramics and building materials, and for research
ingeochemistry, forensic science and archaeology
X-ray Fluorescence
The physics of XRF
When materials are exposed to short-wavelength X-rays or to gamma rays,
ionisation of their component atoms may take place. Ionisation consists of
the ejection of one or more electrons from the atom, and may take place if
the atom is exposed to radiation with the energygreater than its ionisation
potential. X-rays and gamma rays can be energetic enough to expel tightly
held electrons from the inner orbitals of the atom. The removal of an
electron in this way renders the electronic structure of the atom unstable,
and electrons in higher orbitals "fall" into the lower orbital to fill the hole left
behind. In falling, energy is released in the form of a photon, the energy of
which is equal to the energy difference of the two orbitals involved. Thus,
the material emits radiation, which has energy characteristic of the atoms
present. The term fluorescence is applied to phenomena in which the
absorption of radiation of a specific energy results in the re-emission of
radiation of a different energy (generally lower)

Physics of X-ray fluorescence; in a schematic representation

Characteristic radiation

Each element has electronic orbitals of characteristic energy. Following


removal of an inner electron by an energetic photon provided by a primary
radiation source, an electron from an outer shell drops into its place. There
are a limited number of ways in which this can happen, as shown in figure
1. The main transitions are given names: an L→K transition is traditionally
called Kα, an M→K transition is called Kβ, and an M→L transition is called
Lα, and so on. Each of these transitions yields a fluorescent photon with a
characteristic energy equal to the difference in energy of the initial and final
orbital. The wavelength of this fluorescent radiation can be calculated
from Planck's Law:

The fluorescent radiation can be analysed either by sorting the energies of


the photons (energy-dispersive analysis) or by separating the wavelengths
of the radiation (wavelength-dispersive analysis). Once sorted, the intensity
of each characteristic radiation is directly related to the amount of each
element in the material. This is the basis of a powerful technique
in analytical chemistry. Figure 2 shows the typical form of the sharp
fluorescent spectral lines obtained in the wavelength-dispersive method
(see Moseley's law).

Figure 1: Electronic transitions in a calcium atom. Remember,


when electrons are jumping down, one of the electrons in the
lower orbital is missing.

Primary radiation
In order to excite the atoms, a source of radiation is required, with sufficient
energy to expel tightly held inner electrons. Conventional X-ray
generators are most commonly used, because their output can readily be
"tuned" for the application, and because higher power can be deployed
relative to other techniques. However, gamma ray sources can be used
without the need for an elaborate power supply, allowing an easier use in
small portable instruments. When the energy source is asynchrotron or the
X-rays are focussed by an optic like a polycapillary, the X-ray beam can be
very small and very intense. As a result, atomic information on the sub-
micrometer scale can be obtained. X-ray generators in the range 20–60 kV
in order to the K line, which allows excitation of a broad range of atoms.
The continuous spectrum consists of "bremsstrahlung" radiation: radiation
produced when high energy electrons passing through the tube are
progressively decelerated by the material of the tube anode (the "target"). A
typical tube output spectrum is shown in figure 3.

Figure 2: Typical energy dispersive XRF spectrum Figure 3: Spectrum of a rhodium target tube
operated at 60 kV,showing continuous spectrum and K lines

Dispersion
In energy dispersive analysis, the fluorescent X-rays emitted by the
material sample are directed into a solid-state detector which produces a
"continuous" distribution of pulses, the voltages of which are proportional to
the incoming photon energies. This signal is processed by a multichannel
analyser (MCA) which produces an accumulating digital spectrum that can
be processed to obtain analytical data. In wavelength dispersive analysis,
the fluorescent X-rays emitted by the material sample are directed into a
diffraction grating monochromator. The diffraction grating used is usually a
single crystal. By varying the angle of incidence and take-off on the crystal,
a single X-ray wavelength can be selected. The wavelength obtained is
given by the Bragg Equation:

Where d is the spacing of atomic layers parallel to the crystal surface.


Detection
In energy dispersive analysis, dispersion and detection are a single
operation, as already mentioned above. Proportional counters or various
types of solid state detectors (PIN diode, Si(Li), Ge(Li), Silicon Drift
Detector SDD) are used. They all share the same detection principle: An
incoming X-ray photon ionises a large number of detector atoms with the
amount of charge produced being proportional to the energy of the
incoming photon. The charge is then collected and the process repeats
itself for the next photon. Detector speed is obviously critical, as all charge
carriers measured have to come from the same photon to measure the
photon energy correctly (peak length discrimination is used to eliminate
events that seem to have been produced by two X-ray photons arriving
almost simultaneously). The spectrum is then built up by dividing the
energy spectrum into discreet bins and counting the number of pulses
registered within each energy bin. EDXRF detector types vary in resolution,
speed and the means of cooling (a low number of free charge carriers is
critical in the solid state detectors): proportional counters with resolutions of
several hundred eV cover the low end of the performance spectrum,
followed by PIN diode detectors, while the Si(Li), Ge(Li) and Silicon Drift
Detectors (SDD) occupy the high end of the performance scale.
In wavelength dispersive analysis, the single-wavelength radiation
produced by the monochromator is passed into a photomultiplier, a
detector similar to a Geiger counter, which counts individual photons as
they pass through. The counter is a chamber containing a gas that is
ionised by X-ray photons. A central electrode is charged at (typically)
+1700 V with respect to the conducting chamber walls, and each photon
triggers a pulse-like cascade of current across this field. The signal is
amplified and transformed into an accumulating digital count. These counts
are then processed to obtain analytical data.

X-ray intensity
The fluorescence process is inefficient, and the secondary radiation is
much weaker than the primary beam. Furthermore, the secondary radiation
from lighter elements is of relatively low energy (long wavelength) and has
low penetrating power, and is severely attenuated if the beam passes
through air for any distance. Because of this, for high-performance
analysis, the path from tube to sample to detector is maintained under high
vacuum (around 10 Pa residual pressure). This means in practice that most
of the working parts of the instrument have to be located in a large vacuum
chamber. The problems of maintaining moving parts in vacuo, and of
rapidly introducing and withdrawing the sample without losing vacuum,
pose major challenges for the design of the instrument. For less demanding
applications, or when the sample is damaged by a vacuum (e.g. a volatile
sample), a helium-swept X-ray chamber can be substituted, with some loss
of low-Z (Z = atomic number) intensities.

XRF in chemical analysis


The use of a primary X-ray beam to excite fluorescent radiation from the
sample was first proposed by Glocker and Schreiber in 1928. Today, the
method is used as a non-destructive analytical technique, and as a process
control tool in many extractive and processing industries. In principle, the
lightest element that can be analysed is beryllium (Z = 4), but due to
instrumental limitations and low X-ray yields for the light elements, it is
often difficult to quantify elements lighter than sodium (Z = 11), unless
background corrections and very comprehensive interelement corrections
are made.

Energy dispersive spectrometry


In energy dispersivespectrometers (EDX or EDS), the detector allows the
determination of the energy of the photon when it is detected. Detectors
historically have been based on silicon semiconductors, in the form of
lithium-drifted silicon crystals, or high-purity silicon wafers

Figure 4: Schematic arrangement of EDX spectrometer

Si (Li) detectors
These consist essentially of a 3–5 mm thick silicon junction type p-i-n diode
(same as PIN diode) with a bias of -1000 V across it. The lithium-drifted
centre part forms the non-conducting i-layer, where Li compensates the
residual acceptors which would otherwise make the layer p-type. When an
X-ray photon passes through, it causes a swarm of electron-hole pairs to
form, and this causes a voltage pulse. To obtain sufficiently low
conductivity, the detector must be maintained at low temperature, and
liquid-nitrogen must be used for the best resolution. With some loss of
resolution, the much more convenient Peltier cooling can be employed
Figure 5: Schematic form of a Si(Li) detector

Wafer detectors
More recently, high-purity silicon wafers with low conductivity have become
routinely available. Cooled by the Peltier effect, this provides a cheap and
convenient detector, although the liquid nitrogen cooled Si (Li) detector still
has the best resolution (i.e. ability to distinguish different photon energies).
Amplifiers
The pulses generated by the detector are processed by pulse-
shaping amplifiers. It takes time for the amplifier to shape the pulse for
optimum resolution, and there is therefore a trade-off between resolution
and count-rate: long processing time for good resolution results in "pulse
pile-up" in which the pulses from successive photons overlap. Multi-photon
events are, however, typically more drawn out in time (photons did not
arrive exactly at the same time) than single photon events and pulse-length
discrimination can thus be used to filter most of these out. Even so, a small
number of pile-up peaks will remain and pile-up correction should be built
into the software in applications that require trace analysis. To make the
most efficient use of the detector, the tube current should be reduced to
keep multi-photon events (before discrimination) at a reasonable level, e.g.
5–20%.
Processing
Considerable computer power is dedicated to correcting for pulse-pile up
and for extraction of data from poorly resolved spectra. These elaborate
correction processes tend to be based on empirical relationships that may
change with time, so that continuous vigilance is required in order to obtain
chemical data of adequate precision.
Usage
EDX spectrometers are superior to WDX spectrometers in that they are
smaller, simpler in design and have fewer engineered parts. They can also
use miniature X-ray tubes or gamma sources. This makes them cheaper
and allows miniaturization and portability. This type of instrument is
commonly used for portable quality control screening applications, such as
testing toys for Lead (Pb) content, sorting scrap metals, and measuring the
lead content of residential paint. On the other hand, the low resolution and
problems with low count rate and long dead-time makes them inferior for
high-precision analysis. They are, however, very effective for high-speed,
multi-elemental analysis. Field Portable XRF analysers currently on the
market weigh less than 2 kg, and have limits of detection on the order of 2
parts per million of Lead (Pb) in pure sand.
Wavelength dispersive spectrometry
In wavelength dispersivespectrometers (WDX or WDS), the photons are
separated bydiffraction on a single crystal before being detected. Although
wavelength dispersive spectrometers are occasionally used to scan a wide
range of wavelengths, producing a spectrum plot as in EDS, they are
usually set up to make measurements only at the wavelength of the
emission lines of the elements of interest. This is achieved in two different
ways

Figure 6: Schematic arrangement of wavelength dispersive spectrometer

 "Simultaneous" spectrometers have a number of "channels"


dedicated to analysis of a single element, each consisting of a fixed-
geometry crystal monochromator, a detector, and processing
electronics. This allows a number of elements to be measured
simultaneously, and in the case of high-powered instruments,
complete high-precision analyses can be obtained in under 30 s.
Another advantage of this arrangement is that the fixed-geometry
monochromators have no continuously moving parts, and so are very
reliable. Reliability is important in production environments where
instruments are expected to work without interruption for months at a
time. Disadvantages of simultaneous spectrometers include relatively
high cost for complex analyses, since each channel used is
expensive. The number of elements that can be measured is limited
to 15–20, because of space limitations on the number of
monochromators that can be crowded around the fluorescing sample.
The need to accommodate multiple monochromators means that a
rather open arrangement around the sample is required, leading to
relatively long tube-sample-crystal distances, which leads to lower
detected intensities and more scattering. The instrument is inflexible,
because if a new element is to be measured, a new measurement
channel has to be bought and installed.
 "Sequential" spectrometers have a single variable-geometry
monochromator (but usually with an arrangement for selecting from a
choice of crystals), a single detector assembly (but usually with more
than one detector arranged in tandem), and a single electronic pack.
The instrument is programmed to move through a sequence of
wavelengths, in each case selecting the appropriate X-ray tube
power, the appropriate crystal, and the appropriate detector
arrangement. The length of the measurement program is essentially
unlimited, so this arrangement is very flexible. Because there is only
one monochromator, the tube-sample-crystal distances can be kept
very short, resulting in minimal loss of detected intensity. The obvious
disadvantage is relatively long analysis time, particularly when many
elements are being analysed, not only because the elements are
measured in sequence, but also because a certain amount of time is
taken in readjusting the monochromator geometry between
measurements. Furthermore, the frenzied activity of the
monochromator during an analysis program is a challenge for
mechanical reliability. However, modern sequential instruments can
achieve reliability almost as good as that of simultaneous
instruments, even in continuous-usage applications.

Sample presentation
In order to keep the geometry of the tube-sample-detector assembly
constant, the sample is normally prepared as a flat disc, typically of
diameter 20–50 mm. This is located at a standardized, small distance from
the tube window. Because the X-ray intensity follows an inverse-square
law, the tolerances for this placement and for the flatness of the surface
must be very tight in order to maintain a repeatable X-ray flux. Ways of
obtaining sample discs vary: metals may be machined to shape, minerals
may be finely ground and pressed into a tablet, and glasses may be cast to
the required shape. A further reason for obtaining a flat and representative
sample surface is that the secondary X-rays from lighter elements often
only emit from the top few micrometers of the sample. In order to further
reduce the effect of surface irregularities, the sample is usually spun at 5–
20 rpm. It is necessary to ensure that the sample is sufficiently thick to
absorb the entire primary beam. For higher-Z materials, a few millimetres
thickness is adequate, but for a light-element matrix such as coal, a
thickness of 30–40 mm is needed.
Monochromators
The common feature of monochromators is the maintenance of a
symmetrical geometry between the sample, the crystal and the detector. In
this geometry the Bragg diffraction condition is obtained.
The X-ray emission lines are very narrow (see figure 2), so the angles must
be defined with considerable precision. This is achieved in two ways:
Figure 7: Bragg diffraction condition

Flat crystal with Soller collimators


 The Soller collimator is a stack of parallel metal plates, spaced a few
tenths of a millimetre apart. To improve angle resolution, one must
lengthen the collimator, and/or reduce the plate spacing. This
arrangement has the advantage of simplicity and relatively low cost,
but the collimators reduce intensity and increase scattering, and
reduce the area of sample and crystal that can be "seen". The
simplicity of the geometry is especially useful for variable-geometry
monochromators
 Curved crystal with slits

The Rowland circle geometry ensures that the slits are both in focus, but in
order for the Bragg condition to be met at all points, the crystal must first be
bent to a radius of 2R (where R is the radius of the Rowland circle), then
ground to a radius of R. This arrangement allows higher intensities
(typically 8-fold) with higher resolution (typically 4-fold) and lower
background. However, the mechanics of keeping Rowland circle geometry
in a variable-angle monochromator is extremely difficult. In the case of
fixed-angle monochromators (for use in simultaneous spectrometers),
crystals bent to a logarithmic spiral shape give the best focusing
performance. The manufacture of curved crystals to acceptable tolerances
increases their price considerably.
Crystals
 The desirable characteristics of a diffraction crystal are:
 High diffraction intensity
 High dispersion
 Narrow diffracted peak width
 High peak-to-background
 Absence of interfering elements
 Low thermal coefficient of expansion
 Stability in air and on exposure to X-rays
 Ready availability
 Low cost

Crystals with simple structure tend to give the best diffraction performance.
Crystals containing heavy atoms can diffract well, but also fluoresce
themselves, causing interference. Crystals that are water-soluble, volatile
or organic tend to give poor stability.
Commonly used crystal materials include LiF (lithium fluoride), ADP
(ammonium dihydrogen phosphate), Ge (germanium), graphite, InSb
(indium antimonide), PE (tetrakis-(hydroxymethyl)-methane: penta-
erythritol), KAP (potassium hydrogen phthalate), RbAP (rubidium hydrogen
phthalate) and TlAP (thallium (I) hydrogen phthalate). In addition, there is
an increasing use of "layered synthetic microstructures", which are
"sandwich" structured materials comprising successive thick layers of low
atomic number matrix, and monoatomic layers of a heavy element. These
can in principle be custom-manufactured to diffract any desired long
wavelength, and are used extensively for elements in the range Li to Mg.
Detectors
Detectors used for wavelength dispersive spectrometry need to have high
pulse processing speeds in order to cope with the very high photon count
rates that can be obtained. In addition, they need sufficient energy
resolution to allow filtering-out of background noise and spurious photons
from the primary beam or from crystal fluorescence. There are four
common types of detector:
 gas flow proportional counters
 sealed gas detectors
 scintillation counters
 semiconductor detectors

Figure 10: Arrangement of gas flow proportional counter

Gas flow proportional counters are used mainly for detection of longer
wavelengths. Gas flows through it continuously. Where there are multiple
detectors, the gas is passed through them in series, then led to waste. The
gas is usually 90% argon, 10% methane ("P10"), although the argon may
be replaced with neon or helium where very long wavelengths (over 5 nm)
are to be detected. The argon is ionised by incoming X-ray photons, and
the electric field multiplies this charge into a measurable pulse. The
methane suppresses the formation of fluorescent photons caused by
recombination of the argon ions with stray electrons. The anode wire is
typically tungsten or nichrome of 20–60 μm diameter. Since the pulse
strength obtained is essentially proportional to the ratio of the detector
chamber diameter to the wire diameter, a fine wire is needed, but it must
also be strong enough to be maintained under tension so that it remains
precisely straight and concentric with the detector. The window needs to be
conductive, thin enough to transmit the X-rays effectively, but thick and
strong enough to minimize diffusion of the detector gas into the high
vacuum of the monochromator chamber. Materials often used are beryllium
metal, aluminised PET film and aluminised polypropylene. Ultra-thin
windows (down to 1 μm) for use with low-penetration long wavelengths are
very expensive. The pulses are sorted electronically by "pulse height
selection" in order to isolate those pulses deriving from the secondary X-ray
photons being counted.
Sealed gas detectors are similar to the gas flow proportional counter,
except that the gas does not flow though it. The gas is usually krypton or
xenon at a few atmospheres pressure. They are applied usually to
wavelengths in the 0.15–0.6 nm range. They are applicable in principle to
longer wavelengths, but are limited by the problem of manufacturing a thin
window capable of withstanding the high pressure difference.
Scintillation counters consist of a scintillating crystal (typically of sodium
iodide doped with thallium) attached to a photomultiplier. The crystal
produces a group of scintillations for each photon absorbed, the number
being proportional to the photon energy. This translates into a pulse from
the photomultiplier of voltage proportional to the photon energy. The crystal
must be protected with a relatively thick aluminium/beryllium foil window,
which limits the use of the detector to wavelengths below 0.25 nm.
Scintillation counters are often connected in series with a gas flow
proportional counter: the latter is provided with an outlet window opposite
the inlet, to which the scintillation counter is attached. This arrangement is
particularly used in sequential spectrometers.
Semiconductor detectors can be used in theory, and their applications
are increasing as their technology improves, but historically their use for
WDX has been restricted by their slow response.
Extracting analytical results
At first sight, the translation of X-ray photon count-rates into elemental
concentrations would appear to be straightforward: WDX separates the X-
ray lines efficiently, and the rate of generationof secondary photons is
proportional to the element concentration. However, the number of
photons leaving the sample is also affected by the physical properties of
the sample: so-called "matrix effects". These fall broadly into three
categories:

 X-ray absorption
 X-ray enhancement
 sample macroscopic effects

All elements absorb X-rays to some extent. Each element has a


characteristic absorption spectrum which consists of a "saw-tooth"
succession of fringes, each step-change of which has wavelength close to
an emission line of the element. Absorption attenuates the secondary X-
rays leaving the sample. For example, the mass absorption coefficient of
silicon at the wavelength of the aluminium Kα line is 50 m²/kg; whereas that
of iron is 377 m²/kg. This means that a given concentration of aluminium in
a matrix of iron gives only one seventh of the count rate compared with the
same concentration of aluminium in a silicon matrix. Fortunately, mass
absorption coefficients are well known and can be calculated. However, to
calculate the absorption for a multi-element sample, the composition must
be known. For analysis of an unknown sample, an iterative procedure is
therefore used. It will be noted that, to derive the mass absorption
accurately, data for the concentration of elements not measured by XRF
may be needed, and various strategies are employed to estimate these. As
an example, in cement analysis, the concentration of oxygen (which is not
measured) is calculated by assuming that all other elements are present as
standard oxides.
Enhancement occurs where the secondary X-rays emitted by a heavier
element are sufficiently energetic to stimulate additional secondary
emission from a lighter element. This phenomenon can also be
modelled, and corrections can be made provided that the full matrix
composition can be deduced.
Sample macroscopic effects consist of effects of inhomogeneities of
the sample, and unrepresentative conditions at its surface. Samples are
ideally homogeneous and isotropic, but they often deviate from this
ideal. Mixtures of multiple crystalline components in mineral powders
can result in absorption effects that deviate from those calculable from
theory. When a powder is pressed into a tablet, the finer minerals
concentrate at the surface. Spherical grains tend to migrate to the
surface more than do angular grains. In machined metals, the softer
components of an alloy tend to smear across the surface. Considerable
care and ingenuity are required to minimize these effects. Because they
are artifacts of the method of sample preparation, these effects can not
be compensated by theoretical corrections, and must be "calibrated in".
This means that the calibration materials and the unknowns must be
compositionally and mechanically similar, and a given calibration is
applicable only to a limited range of materials. Glasses most closely
approach the ideal of homogeneity and isotropy, and for accurate work,
minerals are usually prepared by dissolving them in a borate glass, and
casting them into a flat disc or "bead". Prepared in this form, a virtually
universal calibration is applicable.
Further corrections that are often employed include background
correction and line overlap correction. The background signal in an XRF
spectrum derives primarily from scattering of primary beam photons by
the sample surface. Scattering varies with the sample mass absorption,
being greatest when mean atomic number is low. When measuring trace
amounts of an element, or when measuring on a variable light matrix,
background correction becomes necessary. This is really only feasible
on a sequential spectrometer. Line overlap is a common problem,
bearing in mind that the spectrum of a complex mineral can contain
several hundred measurable lines. Sometimes it can be overcome by
measuring a less-intense, but overlap-free line, but in certain instances a
correction is inevitable. For instance, the Kα is the only usable line for
measuring sodium, and it overlaps the zinc Lβ (L2-M4) line. Thus zinc, if
present, must be analysed in order to properly correct the sodium value.
A glass "bead" specimen for XRF analysis
being cast at around 1100 °C in a Herzog
automated fusion machine in a cement
plant quality control laboratory. 1 (top):
fusing, 2: preheating the mould, 3: pouring t
he melt, 4: cooling the "bead"

Conclusion
In conclusion, we have to attest our supervisor (Muhammad Mazhar-
ul-Islam who was our senior supervisor and Dr.Yaqoob who was our
departmental incharge for our internship) at PCSIR for the good job.
we really appreciate the way we have been guided through this
internship programme with Engineering, beginning from the
opportunity to take the time we needed to refresh and expand our
knowledge in several issues concerning Electrical queries, over a
somehow protected period where we could discover and learn to
value our new working environment, and finally earned the
confidence to deal with assignments ourselves. It is through them that
we did enjoy our work everyday.

Recommendations

We recommend that PCSIR should once in a while organize a team building


exercises outside Engineering Complex to its staff in order to bring them closer.
This would give staff time to re-examine what they have achieved so far, share
personal experiences and ideas, learn to be together and appreciate the importance
of team work at work.
WE must recommend them for the continued financial support to the interns. We
think it is through there generosity that interns find it abit easy to afford there
meals while at work and meet there daily transport expenses to and from work. It
would be even more generous if PCSIR can review its financial support to interns
to reflect the ever changing economic situation in Pakistan.
From our experience we can wholeheartedly recommend PCSIR internship
programme to everyone who would like to experience an organization that has in
our opinion realized their vision to find the balance between being progressive,
able to balance human concerns, technical considerations and nevertheless being
highly successful. What you have to bring with you, is the willingness to improve
knowledge about the environment, your work experience and you have to be able
to work independently, self motivated and you must solve smaller problems on
your own. Anyhow, if you’ve got into some serious trouble you will always find
somebody assisting you to work it out.