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SWITCHES, RELAYS, AND ANNUNCIATORS

I. SWITCHES
- Same operation with on/off control
- They may be operated by hand, actuated by a mechanical signal, or actuated by a process
or electrical signal.
- They may be used for many things including energizing alarms, interlocks, safety systems,
equipment, or other devices when a process condition meets a preset value.

PHYSICAL SWITCH TYPES

A. Toggle Switches
- They consist of a rocker device, usually a lever, that allows a circuit to be powered or
depowered by throwing the switch from the open to closed position or vice versa.
- They can be made exceptionally durable with metal housings.
- They can be made so that they take up very little room and can be installed in great numbers
on panels.
- With the addition of light indicators that show whether they’re on or off, they’re ideal ways to
control large groups of machines.

Advantages: Disadvantages:
 Typically small footprint  Minimal backlighting options available
 Ideal for use with circuit boards  Restricted labeling options
 Easy to seal  Requires a toggle lock washer
 Highly durable

B. Limit Switches
- They are contact sensing devices widely used for detecting the presence or position of
objects in industrial automation systems.
- They can be installed into machinery as control instruments for standard operations or as
emergency devices to prevent machinery malfunction.

Three Key Components of Limit Switches:


1. Actuator Head – The actuator is the part of the switch that makes physical contact with the
object.
2. Switch Body – The switch body is the component containing the electrical contact
mechanism. The contacts within the body open or close the electrical circuit when the
actuator is activated.
3. Receptacle/Terminals – The component containing the terminal screws or screw/clamp
assembly necessary for wiring purposes.
Advantages: Disadvantages:
 Can be used in almost any industrial Not desirable in food application or areas
environment where repeated touching can damage the
 Very precise in terms of accuracy and object
repeatability Moving mechanical parts will wear out.
 Consume little electrical energy Generally restricted to equipment operating at
 Can switch loads with high inductance relatively low speeds
 Can control multiple loads

C. Proximity Switches
- They sense the closeness of an object without having to make physical contact.
- These switches are non-contact sensors, using magnetic, electric, or optical means to sense
the proximity of objects.
- They are used to measure the position of machine components, security systems, and in
applications such as detecting the opening of a door.

Four Basic Types of Proximity Switches:


1. Inductive – These switches sense distances to objects by generating magnetic fields. They
are similar in principle to metal detectors.
2. Capacitive – These switches sense distance to objects by detecting changes in electrical
capacitance around it.
3. Infrared – These work by sending out beams of invisible infrared light. A photodetector on
the proximity switch detects any reflections of this light. These reflections allow infrared
proximity switches to determine whether there is an object nearby.
4. Acoustic – These sensors use a transducer to transmit inaudible sound waves at various
frequencies in a preset sequence, then measure the length of time the sound takes to hit a
nearby object and return to a second transducer on the switch.

Advantages: Disadvantages:
 They do not cause abrasion or damage  Unlike switches which rely on physical
to the object. contact, proximity sensors are affected
 No contacts are used for output, so it by ambient temperatures, surrounding
has a longer service life. objects, and other sensors.
 Provide high-speed response
compared with switches that require
physical contact

D. Vibration Switches
- They are devices that recognize the amplitude of the vibration to which it is exposed and
provides some sort of response when this amplitude exceeds a predetermined threshold
value.
- They are primarily used for protecting critical machinery from costly destructive failure by
initiating an alarm or shutdown when excessive vibration of the machinery is detected.
- They can also be utilized to warn the absence of vibration, such as when a conveyer ceases
to function due to a broken drive belt.
- They are commonly used on rotating equipment such as compressors, centrifuges, steam
turbines, and blowers.

Advantages:

 Provides continuous machinery protection


 Electronic and mechanical switches are available.
 Adjustable time delays to avoid false trips during switch power up, equipment startup, and
operational changes

E. Process Variable Switches


- Such switches can be used to sound alarms, indicating that a process variable has exceeded
normal parameters, or they can be used to shut down processes or equipment if these
variables have reached dangerous or destructive levels.

Types of Process Variable What process variable does


Sensing Element
Switches it detect?
Pressure Switches Presence of fluid pressure Diaphragms or bellows
Level of liquid or solid in a
Level Switches Floats
vessel
Temperature Switches Temperature of an object Bimetallic strips
Flow Switches Flow of fluid through a pipe Paddles

SYSTEM RESPONSES DUE TO SWITCH ACTION

A. Alarm Switches
- They are used to notify when a process variable enters an abnormal range. The switch
triggers an alarm that informs the process technician of the condition.

“Hard” vs. “Soft” Alarms


Hard alarms Soft alarms
They are hard-wired into the process. They are software-implemented alarms found
within a Distributed Control System (DCS) or a
Programmable Logic Controller (PLC).
They are not exposed to the adverse effects of They can be susceptible to failures that could
a common-mode failure because they maintain disable all soft alarms in the system.
complete independence from the DCS or PLC.
Basic Alarm Trip Functions Trigger
High and Low Limit Alarms When the value of the variable being measured
exceeds a preset high or low alarm trip point
Rate-of-Change Alarm When the input rate-of-change exceeds a user-
selected rate over a user-selected time period
Self-Diagnostic Alarm Some limit alarm trips continuously monitor
their own status during operation, and trip if
they are not operating properly.
Average Alarms When the average of two or three input signals
exceeds a pre-selected high or low trip point.
Differential Alarms When the difference between two input signals
exceeds a specific value
Window Alarm When the process variable is outside of the
low/high trip point ranges.

Alarm Trips with Multiple Relay Outputs Mechanism


 A status change of a single high alarm
occurs when the input rises above the trip
point.
High Alarm  The status will return to a non-alarm
condition when the input falls below the
deadband.

 This alarm accepts one input, but has two


high relays, each with its own trip point.
 When the input rises above Trip Point 1 (the
lower trip point), the first set of contacts will
High/High Alarm change status merely to serve as a warning;
however, should the input rise above Trip
Point 2 (the higher trip point), the second
set of contacts change status, which may
initiate an emergency shutdown.

 The alarm condition of a single low alarm


occurs when the input falls below the trip
point. The status will return to a non-alarm
condition when the input rises above the
Low Alarm deadband.
 A typical application of a low alarm is
warning of a low tank level to avert
problems with a pump running dry.

 A dual low alarm accepts one input, but has


two relays, each with its own independent
Low/Low Alarm trip point.
 When the input falls below Trip Point 1, the
first set of contacts will change status
merely to serve as a warning. Should the
input fall below Trip Point 2, the second set
of contacts change status, possibility
initiating a shutdown of the process.
 A typical application includes monitoring the
low extreme temperature of a cryogenic
tank to avoid over-cooling.
 A dual high/low alarm accepts one input
High/Low Alarm and has two relays, each with a separate
trip point.

B. Shutdown Switches
- They are used to actuate a circuit that shuts down a process. In fail-safe situations, they can
be used to deactivate a circuit or detect an open circuit to shutdown part of the process.

C. Autostart Switches
- They trigger an auto start sequence when predetermined process conditions are met.

D. Bypass Switches
- They allow the user to override (bypass) the normal operation of a system or device in
cases of high inrush or fault conditions.
- Static bypass switches allow the normal uninterruptible power supply (UPS) operation to
be circumvented in cases of an overload or fault situation without loss of power to the load.
- An external maintenance bypass is attached to the outside of UPS and is sometimes
referred to as a wraparound bypass. It allows the engineer to completely remove power
from the system for servicing or removal, without any load interruption.

SWITCH SYMBOLS
Component Circuit Symbol Function of Component
Push Switch A push switch allows current to flow
(push-to- only when the button is pressed. This
make) is the switch used to operate a
doorbell.
Push-to-Break This type of push switch is normally
Switch closed (on), it is open (off) only when
the button is pressed.
On-Off Switch SPST = Single Pole, Single Throw.
(SPST) An on-off switch allows current to flow
only when it is in the closed (on)
position.
2-way Switch SPDT = Single Pole, Double Throw.
(SPDT) A 2-way changeover switch directs the
flow of current to one of two routes
according to its position. Some SPDT
switches have a central off position
and are described as 'on-off-on'.
Dual On-Off DPST = Double Pole, Single Throw.
Switch A dual on-off switch which is often
(DPST) used to switch mains electricity
because it can isolate both the live and
neutral connections.
Reversing DPDT = Double Pole, Double Throw.
Switch This switch can be wired up as a
(DPDT) reversing switch for a motor. Some
DPDT switches have a central off
position.

Relay An electrically operated switch, for


example a 9V battery circuit connected
to the coil can switch a 230V AC mains
circuit.
NO = Normally Open,
COM = Common,
NC = Normally Closed.

II. RELAYS
 They assist in signal transfer by increasing (boosting), passing, or maintaining a signal. It is a
device that initiates action in a circuit in response to some change in conditions in that circuit
or in some other circuit.
 When applied to pneumatic (computational) devices, relays are analog instruments handling
continuously variable signals.
 When applied to electrical devices, relays are discrete, on/off devices.

Types of Relays
A. Pneumatic and Hydraulic
- Used to perform mathematical operations, signal conditioning, and selection or
modification operations.
 Pneumatic Relays – are those which are attached to circuits that conduct
compressed air rather than flow of electrons; however, the principle is the same.
 Hydraulic Relays – this relay uses compressed liquid instead of air.

a. Electronic (on/off Control)


- Used to control one or more circuits that are not normally part of the control circuit.

Advantages of Electronic Relay: Disadvantages of Electronic Relay:


 They require low maintenance.  The high-tension supply is required for
 The relay has fast response time. their operation.
 They decrease the burden on the  The power consumption in the
instrument transformer. electronic relay is very high.
 The relay has the short lifespan.

b. Timing
- May be electrical, mechanical, electromechanical that is used to determine the elapsed
time between the start and stop of related operations or events (e.g. a timing relay may
be used to start an agitator 15 seconds after the pump starts).
- Examples are pneumatic timers, electronic timers, and motor-driven timers.

c. Pneumatic Booster
- Contains a high-pressure or volume source that increases the signal value or volume.
- Advantages:
 Quick response with increased actuator stroking speeds
 Maintains correct actuator positioning at high stroking speeds
 Adjustable by pass valve provides good operational sensitivity
 High stability which allow normal slow actuator response to slow signal changes
 Capable of using high pressure plant air supply
 Different Booster sizes available to suit wide range of actuator sizes
 Main internal air supply valve with soft seat insert for tight shut off

d. Selection
- Can take two or more inputs and chose a predetermined value (e.g. high, medium, low).

Relay Applications
 Refrigerator – This appliance has motors and fans. Relays are responsible in controlling
these parts so that refrigerator work and produce cold temperature.
 Controlling traffic lights – They can be operated remotely with the use of a switching
component.
 Automatic garage door –The door’s movement and direction are the ones being controlled.
 Long telegraph lines – The weak signal received at an intermediate station could control a
contact, regenerating the signal for further transmission.

III. ANNUNCIATORS
 They are instruments that provide audible and/or visual alarms in reference to some
measured variable.
 They can be standalone panel board devices or configured as part of a distributed control
system (DCS).
 The purpose of an alarm system (annunciator) is to bring attention to an abnormal or unsafe
operating condition in the plant. Traditional annunciators used discrete alarm modules for
this purpose.
 They are used in installations where simplicity is desired or where separation from the basic
process control system is required for safety reasons.
 The annunciator system consists of multiple alarm points. Each alarm circuit includes a
problematic contact (alarm switch), a logic module and a visual indicator. The problem
contact is an alarm switch that monitors a particular process variable and is activated when
the variable exceeds the preset limits.
 Examples of Annunciators:
o Audible Annunciators – bell, chime, horn, loudspeaker, and sire
o Visible Annunciators – indicator light, strobe light, and rotating beacon
FINAL CONTROL ELEMENT
INTRODUCTION
A final control element is defined as a mechanical device that physically changes a process in
response to a change in the control system setpoint.
Final control elements are also defined as devices that complete the control loop. They link the
output of the controlling elements with their processes.

COMPONENTS/PARTS OF A CONTROL VALVE


 Bonnet – contains the packing box that provides a seal around the sliding stem
mechanism that connects the actuator to the valve plug.
 Plug (disc or ball) – plug assembly that includes the valve stem moves to open or close
the flow path through the valve.
 Actuator – the device that provides motion to the valve using a spring diaphragm, spring
piston, or double-acting piston.
 Stem – is the pushing and pulling rod that transfers the motion of the actuator to the valve
plug.
 Seat – the stationary part of the valve trim connected to the body that comes in contact
with the valve plug.
 Spring – provides the energy to move the valve in the opposite direction of the diaphragm
loading motion.
 Diaphragm – the flexible member that creates a force to move the stem.

 Valve Positioner – A valve positioner is actually a proportional-only controller. The


position of the valve stem is then compared to the value of the instrument signal and a
response is produced to make the position of the valve and the signal equal
 Handwheel – an actuator accessory that is used to manually override the actuator or to
limit its motion.
 I/P or current – to – pneumatic transducer – a device that converts a milliampere signal
into a pneumatic pressure. The most common use for an I/P transducer is to provide the
source of energy needed to drive a diaphragm or piston actuator.

CONTROL VALVE FAILURE CONDITIONS

Control valves are ultimately responsible for regulating the movement of fluids in a process, if
there is a power or air failure they should move to safe position. Design Engineers should
address possibilities with each control valve placed into the process.
TYPES OF CONTROL VALVES: LINEAR

Type of Linear Control Valve Description Advantages Disadvantages

1. Globe Valve

 Single Seated  Large amount of  Simple design  More


force required to  Simplified complex
drive the stem maintenance designs
 Used for  Smaller and required for
controlling large lighter balancing
range of process  Good shutoff
parameters
hence used in oil
and gas
production,
power
generation
 Double Seated  Use opposing  Reduced actuator  Poor
forces from the force due to shutoff.
two plugs to balancing.  Heavy and
minimize the  Action easily bulky.
actuator force changed  More parts
required for (Direct/Reverse). to service.
control  High flow  Only semi-
movement capacity. balanced.
 Used for high
flow and high
pressure services
 Split Body  Useful in  High flow  More
services where a capacity expensive
flow stream  Valve used for
must be diverted mixing and
(split) between diverting liquids
two different  Leakage
directions, or capability with
where two flow normal single
streams must seated globe
converge (mix) valve
within the valve
to form a single
flow stream
 Used in textile
industry

 Cage-guided Globe  A more modern  the valve’s  tend to leak


Valves version of the flowing more when
globe valve characteristics in the shut
design uses a may be easily position
piston-shaped altered just by due to a
plug inside a replacing the greater
surrounding cage cage with number of
with ports cast or another having leak paths
machined into it different size or
shape of holes
 the cage can
modify the flow
2. Y-style valves  The seat and  allow the fluid to  high
stem are angled pass through pressure
at approximately without drop
45° to the pipe difficulty and
axis minimizes fluid
 Used in high clogging/
pressure and corrosion in the
other critical long term
services where
pressure drop is
concerned.

3. Pinch/Diaphragm Valves
 Pinch Valve  valve with a  extremely clean  can not be
flexible  leak proof seal used in high
elastomer body  tight shut off temperature
that can be  low s ( -60 to
pinched maintenance 450F)
 Applications: repairs can be  can only be
medical, made without used in
pharmaceutical, interrupting the moderate
wastewater, pipeline pressures
slurries, pulp,  used in (approximat
powder, pellets corrosive and ely 300 psi)
 Diaphrahgm Valve  valve with a abrasive
flexible services
disc/diaphragm
which comes
into contact with
a seat at the top
of the valve
body to form a
seal
 Applications:
pharmaceutical,
food processing,
and water
treatment
industries

4. Gate Valves  designed to  available in  erosion of


minimize large sizes the seat and
( also known as knife valves or pressure drop  inexpensive disk can
slide valves) across the valve  bidirectional occur
in the fully  low pressure  poor
opened position drop throttling
and stop the flow  used as shut-off characteristi
of fluid valve cs
completely  difficult to
 Applications: oil repair
and gas industry,  slow open
pharmaceuticals, and close
manufacturing, time
automotive,  can’t be
marine used in
sanitary
applications
TYPES OF CONTROL VALVES: ROTARY
Rotary Valves have a closure member that moves with rotary motion to modify the rate
of flow through the valves. They are named after the shape of their closure member.

Type of RCV Description and Disadvantage


Advantage
Usages
Butterfly Valves  Closure member  Simple & Light  Part of the disc
is a circular disc construction always faces the
or vane its pivot  Minimum flow
axis at the right obstruction for  Cavitation and
angles to the flowing media choked flow
direction of flow  High Flow  Disc movement
in the pipes. Capacity guides and
 Used to control  Tight shut off affected by flow
all types of fluids with rubber turbulence
including both sleeves
liquids and gases  Requires less time
 Used in steel, to open or close
sugar and textile  Low-pressure
industries drop and high
(containing slurry pressure recovery
particles)
 Used for on-off
control
application

Ball Valves  Closure member  Tight shut off  Poor throttling


shape is like a with minimum characteristics
ball with a port obstruction for  When used in
for fluid flows the flowing media fluids containing
 Used in shut-off  High flow slurries it can
and throttling capacity stick in position
applications  Easily access the and become
 Used in paper, seats when a jammed.
pulp and textile valve requires
industries fixing

TYPES OF VALVE ACTUATORS


Valve Actuators
 A device that responds to an applied instrument signal by creating a linear or rotational
motion.
 What makes a valve a control valve.
 Provides the motion necessary to throttle the valve.
Types of Valve Actuators:
1. Pneumatic Valve Actuators
 Adjust the valve position by converting air pressure into linear or rotary motion.
 The most popular type of valve actuators.
Two main form: Piston actuators and Diaphragm actuators.

 Spring and Diaphragm Actuator


 has a single diaphragm supported by a diaphragm plate connected to a
steel rod called a stem.
 A spring is placed on the opposite side of the plate to create an opposing
return force.
 Advantage – low cost, high mechanical, and excellent throttling control
with or without positioner.
 Piston Actuator
 Have a longer strokes and can
accept much higher input
pressures.
 Compressed air is applied to a
solid piston contained within a
solid cylinder.
 Many of this type are double
acting – air can be fed into
either side of the piston since
there’s no return spring.

2. Hydraulic Valve Actuators


 Convert fluid pressure into motion in response to a signal.
 Advantage – high pressure, very high dynamic stiffness, fast stroking speed and
good frequency response.
 Disadvantage – high initial cost and more difficult maintenance.

 Electrohydraulic Actuators
 Have similar performance characteristics and cost/maintenance
ramifications, except that they contain their own electric-powered
hydraulic pump.
 Main application is remote sites without an air supply when a fail-safe
spring return is needed.
3. Electric Valve Actuators
 An actuator that is powered by a motor that converts electrical energy into
mechanical torque.
Electromechanical Actuators
 driven by an electric motor
 offer the strength of hydraulic actuators with more precise movement and
motion control
 Are programmable, the force and motion profile can be changed in
software without having to shut down and reconfigure the machine.
4. Manual Valve Actuators
 Employs levers, gears, or wheels to move the valve stem.
 Done by a human driving force
 Advantage- inexpensive, typically self-contained, and easy to operate.

 Handwheel Fixed to Stem


 Provide only the mechanical advantage on the wheel.
 When exposed to high temperatures, valve binding makes operation
difficult.
 Hammer Handwheel
 Moves freely through a portion
of its turn and then hits against a lug on a secondary
wheel which is attached to the valve stem.
 Manually-operated Gearbox

 Used if additional mechanical advantage is


necessary for a manually-operated valve

CONTROL VALVE ACCESSORIES


Control valve accessories helps in order to ensure accuracy, boost output, make various control
system components compatible with one another, and to provide layers of safety.
1. Positioner - Its primary function is to accurately position the throttling element within a
control valve as directed by a signal from the process control system.
2. Limit switch (position switch) - Limit switches are used to indicate when a control valve has
reached a specific position. They are used most often to indicate the fully open or fully closed
position, but can be set at intermediate points if desired.
3. Volume booster - A volume booster is a mechanical relay that amplifies the flow of air. It
provides a 1:1 amplification of flow while keeping the output pressure as close as possible to
signal pressure. Since the booster has a separate supply connection, it is not limited by the
capacity of the devices ahead of it in loop.
ANALYTICAL INSTRUMENTS

Gas analyzer is an instrument which is capable of analyzing the species of chemical gases is
present in the sample. Not only it identifies the species but it also has capability to give
measurement value of the quantity which it displays either in numerical form or shows it
graphically.

TYPES OF GAS ANALYZER


 INFRARED GAS ANALYZER

It is used to measure the quantity of various gas. The amount of gas is determined by amount of a
particular frequency of light absorbed by the gas when the light is passed through the gas.
Different molecules in the air absorb different frequencies of light, measuring the absorbed
frequency clearly gives the relation to the amount of particular gas in the air.
Two types:
• Dispersion infrared analyzers - used in laboratories as spectrophotometers
• Non-dispersion infrared analyzers- used for continuous measurement in industrial
applications specifically for measuring the concentration of carbon oxides (CO & CO2).
Advantages:
• Gas molecule doesn’t interact directly with the gas.
• Non-destructive analysis.
• Standard detectors for the measurement of gas in any given environment.
• Monitors emission levels over longer periods of time.
Disadvantages:
• simple measurement becomes a complex measurement
• Higher cost of measuring gas normalization parameter is greater than the cost of primary
dust measurement

 ULTRAVIOLET (UV) GAS ANALYZER

It is a radiant energy (optical) analyzer that uses ultraviolet region of the electromagnetic
radiation spectrum. The UV radiation will pass through the gas inside the gas cell then to the
measurement detector. Thermopiles are used as detectors. The simplest style of non-dispersive
analyzer uses a single light source, shining continuously through a single gas cell, and eventually
falling on a small thermopile which converts the received UV light into heat, and then into a
voltage signal.

Advantages and Disadvantages:


Separate measurements of NO and NO2 eliminate any need for the traditional converters that
have seen frequent use. Using ultraviolet minimizes several maintenance issues. With ultraviolet,
there is no converter and no need to use a chemiluminescent type of analyzer. Using a UV
analyzer in real time gives the user a view of NO2 and NO without the converter. With the
higher levels of NO and NO2, infrared can be effective, but on lower levels, ultraviolet adds
accuracy. But in general, the values given by the IR are more specific than the UV gas analyzer.
There are two general approaches to monitoring emissions from stack gases: In – situ analysis or
extractive analysis.

1. IN – SITU GAS ANALYZER

In-situ analyzers have sensors to take measurements directly in the gas stream. This allows for a
reading without any time delay. In-situ analyzers contain infrared , ultraviolet , or
electrochemical sensors. The analyzer probe sits directly in the gas stream, and the probe sensors
detect the concentration of the species of interest. For this particular in-situ analyzer, the
concentration of the species is measured by using a spectrometer and a xenon flash light beam.
The analyzer units can be configured to relay this information to a variety of devices, such as
computers, strip charts, or modems. A purge air unit is included to keep the sensors from
overheating and prevent contamination.

Advantages and Disadvantages:


In situ gas analyzer is usually small. It is used for direct measurements which saves time and
gives greater accuracy but needs to be calibrated. This can be used in a lot of pipe sizes and flow
rates but the probes and sensor should be designed to function at gas stream temperature and
pressure.

2. EXTRACTIVE GAS ANALYZER:

In extractive measurement a gas sample is taken from the stream, prepared and then evaluated.
Composition of the gas stream sample is determined using one of three sensors: infrared ,
ultraviolet , or electrochemical.
Two ways of sample taking:
• Full Extractive Method- Measurements made can be done either with the moisture still
present in the sample called hot or wet basis or, with a 'dried' sample called cool or dry
basis.
• Dilution Extractive Method- It extracts a very small representative portion of a gas
stream and very accurately dilutes the sample with air before transportation to an
analyser.
Two ways of dilution:
In-stack dilution- dilution of gas sample takes place within the sample probe itself or
dilution mechanism is part of the probe.
Out of stack dilution- dilution takes place after the probe, right at it’s discharge
Advantages
• Can detect extremely low concentrations.
• Many applications possible.
• Can handle a variety of flow rates and pipe sizes.

Disadvantages
• Larger than in-situ analyzers.
• Delayed analysis of gas because it must pass from stream to sample unit to analyzing
unit.
• Analyzers must be calibrated to specific ranges.
SPECTROMETERS
- Instruments that measure or analyse a range of a given characteristic or wavelength of
a substance

1. SPECTROPHOTOMETER
- An optical device that measures the concentration or particles in a solution.
- Light with a pre-selected wavelength is allowed to pass through the sample. The
amount of light absorbed will be determined. The amount of light absorbed increases
with the increase in amount of particles present in the sample.

 Beer’s Law – also referred to as Beer-Lambert law or the Bouguer-Beer law. It was
named after August Beer. It states that the quantity of light directly proportional to the
concentration of the substance and the path length of the light through the solution.
A=εcl
where A is the absorbance, c is the, l is the path length, and ε is a constant of
proportionality known as the molar extinction coefficient.
 Single-beam instrument - the absorbance of control is determined followed by the
sample
o Advantages: low cost, high throughput and high sensitivity
o Disadvantages: prone to drift, dilution is required

 Double-beam spectrophotometers - the light beam is split into two beams by means of
mirrors. One light path goes through the sample chamber and the other light beam passes
through what is referred to as the reference cell or chamber
o Advantages: less prone to drift
o Disadvantages: high cost, low sensitivity, dilution is required

 Components of a spectrophotometer
o Radiant Source
 Ultraviolet Radiation - hydrogen lamp, deuterium lamp
 Visible Radiation - Tungsten filament lamp, carbon arc
 Infrared Radiation - Nernst glower
o Monochromator -breaks polychromatic radiation into component wavelength. The
types of prisms usually employed in commercial instruments are a 60° cornu
quartz and a 30° Littrow prism.
 Diffraction Grating – used in pairs
 Ruled Gratings
 Holographic Gratings
 Prisms

o Transport Vessels (cuvettes) – sample containers


o Detection Devices
 High sensitivity to allow the detection of low levels of radiant energy
 Short response time
 Long-term stability
 An electric signal which is easily amplified for a typical readout apparatus.
o Amplification and Read-out – amplifiers, ammeters, potentiometers and
potentiometric recorder
 Applications of a spectrophotometer
o Qualitative Analysis
o Quantitative Analysis
o Enzyme Assay
o Molecular Weight Determination
o Other Physiochemical Studies
 Heats of formation of molecular addition compound and complexes in
solution
 Determination of empirical formula
 Formation constants of complexes in solution
 Hydration equilibrium of carbonyl compounds
 Association constants of weak acids and bases in organic solvents
 Protein-dye interactions
 Chlorophyll-Protein complexes
 Vitamin-A aldehyde–Protein complex
 Determination of reaction rates
 Dissociation constants of acids and bases
 Association of cyanine dyes

2. Mass Spectrophotometer
- Developed by Francis William Aston
- Identifies the chemical composition of a sample based on the mass-to-charge ratio of
charged particles and identifies the isotopic composition of its constituents
- Determines the structure of the compound by observing its fragmentation
 Applications
o Isotope ratio MS: Isotope Dating and Tracking
o Trace Gas Analysis
o Atom Probe
o Pharmacokinetics
o Protein Characterization
o Space Exploration
 Advantages
o Sensitive
o Excellent toll for identifying unknown components in a sample or confirming
their presence
 Disadvantages
o Cannot identify hydrocarbons that produce similar ions
o Unable to tell optical and geometrical isomers apart
o Cannot distinguish components with the same molecular formula
o Cannot distinguish between isomers of a compound having the same charge-to-
mass ratio

3. Infrared (IR) Spectrophotometer


- Deals with the infrared region of the electromagnetic spectrum
- Analyzes samples based on reflection, emission and absorption
- The two main components are
o Sources – Nernst glower –a rod of a sintered mixture of the oxides of
Zirconium, Ytterbium and Erbium.
o Prism - Sodium chloride or other alkali metal halides are the best material to
form prism and cell container
o Cell container
o Detector – converts IR energy to electrical energy and is amplified by an
amplifier
 Applications
o Identification of functional group and structure elucidation
o Identification of structure substances
o Study of the progress of a chemical reaction
o Detection of impurities via infrared
o Quantitative analysis
 Advantages
o Provides qualitative and quantitative analysis without destroying the sample
o The sample does not need any particular preparation
o Very sensitive, thus, it requires a minimum sample quantity
o Solid, liquid, gases, and semi-solid samples can be analyzed
o Peak intensities, peak positions, peak widths, shapes, and functional groups
provide all helpful information
 Disadvantages
o Difficult handling procedures and maintenance of the sample cells
o There are no infrared spectra in atoms or monoatomic ions
o Requires very sensitive and properly tuned devices
o Aqueous solutions and complex mixtures are complicated to analyze via IR
spectroscopy

In early 1900s, Gas chromatography (GC) was discovered by Mikhail Semenovich


Tsvett as a separation technique to separate compounds. Gas chromatograph uses a flow-through
slender tube called the column, through that totally different chemical constituents of a sample
pass in an exceedingly gas stream (carrier gas, mobile phase) at totally different rates counting
on their varied chemical and physical properties and their interaction with a selected column
filling, referred to as the stationary part.
Instrumental components
Carrier gas
The carrier gas should be with chemicals inert. Ordinarily used gases embody atomic
number 7, helium, argon, and CO2. The selection of carrier gas is usually dependent upon the
kind of detector that is employed. The carrier facility additionally contains a molecular sieve to
get rid of water and alternative impurities.
Sample injection port
For optimum column potency, the sample mustn't be large, and may be introduced onto
the column as a "plug" of vapor - slow injection of enormous samples causes band broadening
and loss of resolution.
Column
There are a unit 2 general styles of column, packed and capillary (also referred to as
open tubular). Packed columns contain a finely divided, inert, solid support material (commonly
supported diatomaceous earth) coated with liquid stationary part. Most packed columns area unit
one 0.5 - 10m long and have an interior diameter of two - 4mm.
Column temperature
For precise work, column temperature should be controlled to at intervals tenths of a
degree. The optimum column temperature is dependent upon the boiling purpose of the sample.
As a rule of thumb, a temperature slightly on top of the typical boiling purpose of the sample
ends up in associate extraction time of two - half-hour.
Detectors
There are several detectors which may be employed in gas activity. Totally different
detectors can offer differing kinds of property. The response of a mass flow dependent detector is
unaffected by make-up gas. Have a glance at this tabular outline of common rate detectors

Applications
 Identification of the oil elements by GC/MS
 Skin samples analysis

Environmental monitoring

 Food, beverage, flavor and fragrance analysis


 Forensic and criminal cases
 Biological and pesticides detections
 Security and chemical warfare agent detection
 Astro chemistry and Geo chemical Research
 RNA isolation
Limitations
1. Not suitable for detecting semi-volatile compounds
2. Only indicates if volatile organic compounds are presents.
3. High concentration so methane is required for higher performance.
4. Frequent calibrations are required.
5. Units of parts per million range
6. Environmental distraction, especially water vapour.
7. Strong electrical fields Rapid variation in temperature at the detector and naturally
occurring compounds may affect instrumental signal.

I. High performance liquid chromatography


High Performance Liquid Chromatography (HPLC) is a form of column
chromatography that pumps a sample mixture or analyte in a solvent (known as the mobile
phase) at high pressure through a column with chromatographic packing material (stationary
phase).
Instrumentation
Main components in an HPLC system include the solvent reservoir, or multiple
reservoirs, a high-pressure pump, a column, injector system and the detector.
The column and the solvent
Confusingly, there are two variants in use in HPLC depending on the relative polarity of
the solvent and the stationary phase.
Normal phase HPLC
It is described as "normal", it isn't the most commonly used form of HPLC. The column
is filled with tiny silica particles, and the solvent is non-polar - hexane, for example. A typical
column has an internal diameter of 4.6 mm (and may be less than that), and a length of 150 to
250 mm.
Reversed phase HPLC
In this case, the column size is the same, but the silica is modified to make it non-polar
by attaching long hydrocarbon chains to its surface - typically with either 8 or 18 carbon atoms
in them. A polar solvent is used - for example, a mixture of water and an alcohol such as
methanol. Reversed phase HPLC is the most commonly used form of HPLC.

A flow scheme for HPLC:


Injection of the sample
Injection of the sample is entirely automated; it is not the same as in gas
chromatography because of the pressures involved
Retention time
The time taken for a particular compound to travel through the column to the detector is known
as its retention time. This time is measured from the time at which the sample is injected to the
point at which the display shows a maximum peak height for that compound.
The detector
There are several ways of detecting when a substance has passed through the column. A
common method which is easy to explain uses ultra-violet absorption.
Interpreting the output from the detector
The output will be recorded as a series of peaks - each one representing a compound in
the mixture passing through the detector and absorbing UV light.
Peaks are also use a another way of measuring the quantities of the compounds present.
Let's suppose that you are interested in a particular compound, X.
The area under the peak is proportional to the amount of X which has passed the
detector, and this area can be calculated automatically by the computer linked to the display. If
the solution of X was less concentrated, the area under the peak would be less - although the
retention time will still be the same.

Other HPLC types:


 Ultra high performance liquid chromatography (UHPLC):
Where standard HPLC typically uses column particles with sizes from 3 to 5µm and
pressures of around 400 bar, uHPLC use specially designed columns with particles down to
1.7µm in size, at pressures in excess of 1000 bar.
 Fast protein liquid chromatography (FPLC)
FPLC is a system similar to high-performance liquid chromatography that is used to
separate or purify proteins and other biomolecules from complex mixtures.

Advantages and Disadvantages


 Speed, efficiency and accuracy
Compared to other chromatographic techniques, such as TLC, HPLC is extremely quick
and efficient. It uses a pump, rather than gravity, to force a liquid solvent through a solid
adsorbent material, with different chemical components separating out as they move at different
speeds.
 Cost and complexity
Despite its advantages, HPLC can be costly, requiring large quantities of expensive
organics. Techniques such as solid phase extraction and capillary electrophoresis can be cheaper
and even quicker, especially for analysis under good manufacturing practice.
 Sensitivity and resolution
In general, HPLC is versatile and extremely precise when it comes to identifying and
quantifying chemical components. With many steps involved, the precision of HPLC is largely
down to the process being automated and therefore highly reproducible.

II. Thin layer chromatography

Thin layer chromatography (TLC) is used to separate the components of a mixture using
a thin stationary phase supported by an inert backing. TLC is an analytical tool widely used
because of its simplicity, relative low cost, high sensitivity, and speed of separation. The goal of
TLC is to obtain well defined, well separated spots.

 Plates (stationary phase)


Silica gel and alumina are among the most common stationary phases, but others are
available as well. Many plates incorporate a compound which fluoresces under short-wave UV
(254 nm). The properties of your sample should be considered when selecting the stationary
phase.
 Solvent (mobile phase)
Proper solvent selection is perhaps the most important aspect of TLC, and determining
the best solvent may require a degree of trial and error. As with plate selection, keep in mind the
chemical properties of the analytes. Varying the ratio can have a pronounced effect of Rf
(Retention factor)
Rf values:
Measurements are often taken from the plate in order to help identify the compounds
present. These measurements are the distance travelled by the solvent, and the distance travelled
by individual spots.
The Rf value for each dye is then worked out using the formula:

How does thin layer chromatography work?

The stationary phase - silica gel:


Silica gel is a form of silicon dioxide (silica). The silicon atoms are joined via oxygen
atoms in a giant covalent structure. However, at the surface of the silica gel, the silicon atoms are
attached to -OH groups. The surface of the silica gel is very polar and, because of the -OH
groups, can form hydrogen bonds with suitable compounds around it as well as van der Waals
dispersion forces and dipole-dipole attractions.

What separates the compounds as a chromatogram develops?


As the solvent begins to soak up the plate, it first dissolves the compounds in the spot
that you have put on the base line. The compounds present will then tend to get carried up the
chromatography plate as the solvent continues to move upwards.
How fast the compounds get carried up the plate depends on two things:
 How soluble the compound is in the solvent. This will depend on how much attraction
there is between the molecules of the compound and those of the solvent.
 How much the compound sticks to the stationary phase - the silica gel, for example. This
will depend on how much attraction there is between the molecules of the compound and
the silica gel.
Common Problems in
TLC:
There are common problems in TLC that should be avoided. Normally, these problems
can be solved or avoided if taught proper techniques.
 Over-large Spots: Spotting sizes of your sample should be not be larger than 1-2 mm in
diameter. The component spots will never be larger than or smaller than your sample
origin spot.
 Uneven Advance of Solvent Front: Uneven advance of the mobile phase is a common
problem encountered in TLC. Consequences would be inaccurate Rf values due to the
uneven advance of sample origin spots. This uneven advance can be caused by a few
factors listed below.
o No flat bottom. When placing the TLC plate into the chamber, place the bottom of
the plate on the edge of the chamber (normally glass container (e.g. beaker)) and
lean the top of the plate along the other side of the chamber. Also, make sure that
the TLC plate is placed in the chamber evenly. Do not tilt the plate or sit it at an
angle.
o Not enough solvent. There should be enough solvent (depends on size of
chamber) to travel up the length of the TLC plate.
o Plate is not cut evenly. It is recommended that a ruler is used so that the plate is
cut evenly.

Advantages and Disadvantages


 The solvents for the TLC plate can be changed.
 TLC can be used to ensure purity of a compound.
 Identification of most compounds can be done simply by checking Rf literature values.
 TLC plates do not have long stationary phases.
 Detection limit is a lot higher.
 TLC operates as an open system.
HUMIDITY

- measure humidity by sensing


changes in physical or electrical - relative humidity - ±5 percent - Operating Temp:
A. Hygrometers
properties in materials due to their from 20-90 accuracy <70℃
moisture content.

- made by attaching thin strips of


wood to thin metal strips forming a
laminate. The laminate is formed
1. Laminate into a spiral or a helix.
Hygrometers
- As the humidity changes, the spiral
flexes, due to the change in the
length of the wood.

- made using human hair.

2. Hair - The change in length can be used - simplest


Hygrometers to control a pointer for visual hygrometer type
readings or a transducer for an
electrical output.

3. Resistive - consist of two electrodes with


Hygrometers/ interdigitated fingers on an
Resistive insulating substrate. The electrodes
Humidity are coated with a hydroscopic
Sensors material (one that absorbs water
such as lithium chloride)

4. Capacitive - uses the change of the dielectric - good longevity


Hygrometers constant of certain thin polymer films of device
that change linearly with humidity,
so that the capacitance between two - fast response
plates using the polymer as the time
dielectric is directly proportional to -working temp: 0-
humidity. 100oC

- use two piezoelectric crystal


5. oscillators; one is used as a
Piezoelectric/ reference and is enclosed in a dry
Sorption atmosphere, and the other is
Hygrometers exposed to the humidity to be
measured.

B. Psychrometers - use the latent heat of vaporization


to determine the relative humidity
- frame holding both the dry and wet
1. Sling
bulb thermometers that can rotate
Psychrometer
about a handle.
- pharmaceutical
and raw material
industries
- works by first cooling the air or gas
until water condenses on an object - building services
C. Dew Point
Measuring Devices and then measuring the temperature engineering
at which condensation takes place (HVAC)

- clean rooms as
well as in
production and
process
technologies

D. Moisture Content
Measuring Devices

- microwaves (1 to 100 GHz) are


absorbed by the water vapor. The
1. Microwave relative amplitudes of the
Absorption transmitted and microwaves passing
through a material are measured.
The ratio of these amplitudes is a
measure of the humidity content of
the material.

- An infrared beam is directed onto


the material and energy of the
reflected rays is measured. The
2. Infrared measured wavelength and
Absorption amplitude of the reflected rays are
compared to the incident
wavelength and amplitude. The
difference between the two is
related to moisture content.

DENSITY/ SPECIFIC GRAVITY

- consists of a graduated glass tube, - Breakable


- Simple Method
A. Hydrometers with a weight at one end, which Glassware
causes the device to float in an - Quick
- Very small
upright position. Measurement measuring range

- sinks in a liquid until an equilibrium - Inexpensive - Limited Accuracy


point between its weight and
buoyancy is reached. - specific - Large volume
weight/ density is read directly from sample required
the tube graduations.

- reading
accuracy
- combination of hydrometer and improved
B. through
thermometer that measures specific
Thermohydrometers corrections from
weight/density and temperature.
lookup tables for
temperature
variations
- converts specific weight/ density of
a liquid into an electrical signal.

- In this case, a fixed volume of


liquid set by the overflow tube is
used
C. Induction
Hydrometers - has a soft iron or similar metal core
attached. As the density/specific
weight of the liquid changes, the
buoyant force on the displacement
device changes. This movement can
be measured by the coil and
converted into a density reading.
- alternate method

- fluid is passed through a U tube


which has a flexible mount so that it
can vibrate when driven from an
D. Vibration outside source. The amplitude of the
Sensors vibration decreases as the specific
weight or density of the fluid
increases, so that by measuring the
vibration amplitude the specific
weight/density can be calculated.

VISCOSITY

- low-viscosity
- uses the principle that an object, substances
when dropped into a liquid, will in pharmaceutical,
- Limited to
descend to the bottom of the vessel food, chemical and
Newtonian fluids
at a fixed rate; the rate of descent is mineral oil
- Small and
A. Falling-Cylinder determined by the size, shape, industries Restricted to
portable
Viscometer density of the object, and the density translucent fluids
and viscosity of the liquid. - Specific
- Easy operation (need to be able
examples: liquid
to see the object's
- higher viscosity = longer time for hydrocarbons,
movement)
object to reach the bottom of the sugar solutions,
vessel. solvents, and
polymer solutions

- consists of a cylindrical, serrated, - measuring


B. Rotating-Disk
metal disk surrounded by a die material viscosity
Viscometer/
chamber where the rubber is and scorch time
Mooney machine pressed with 2500 pounds of force. for rubber before
The rubber is then warmed for two vulcanization.
minutes. Next, the serrated disk is
rotated, in one direction only, at a
speed of 2 revolutions per minute,
while the torque required to rotate
the disk is recorded. The torque
decrease per time can be directly
related to viscosity.

- to measure the
viscosity of oils,
C. Saybolt - control the heat of the fluid and the syrups, varnish,
Instrument/ Efflux viscosity is the time it takes the fluid paints and
Cup Viscometers to fill a 60cc container. Bitumen
emulsions in
industries.

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