Академический Документы
Профессиональный Документы
Культура Документы
Indutrial Research
Acknowledgemen
t
Introduction
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.
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.
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.
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.
Leather Technology
Bacterial bating agents.
Industrial leather processing technology.
Processes for garment leather, shoe upper, sole leather, etc.
Leather auxiliaries and chemicals.
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
Engineering
Design and development of precision machines and machine tools, jigs, moulds, dies and
spare parts of high precision.
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.
Home wiring
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
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.
Outlet slots
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
Safety
Grounding
Fuses
Summary
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:
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.
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.
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:
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 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.
Advantages
Synchronous motors have the following advantages over non-synchronous
motors:
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.
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.
9. Remove the slide from the X-ray holder, place new slide in
holder, record identification, and follow operational steps as
outlined above.
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.
Characteristic radiation
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:
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.
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
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
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
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
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