AIR SEPERATION PLANT (NITROGEN PLANT)

PRINCIPLES OF AIR SEPERATION UNIT

Air separation by rectification in a single/double column using his air liquefaction
principle as a basis, Carl von Linde constructed the first air separation plant for oxygen
production in 1902 using a single-column rectification system. In 1910, he established the
basis for cryogenic air separation with the development of a doublecolumn rectification
system. Now it was possible to produce pure oxygen and pure nitrogen simultaneously.
This involves installing a pressure column below the low-pressure column. At the top of
this pressure column, pure nitrogen was drawn off, liquefied in a condenser and fed to the
top low-pressure column as reflux. At the top of the low-pressure column, pure gaseous
nitrogen was withdrawn, while liquid oxygen evaporated at the bottom of this column to
deliver pure gaseous oxygen. This principle of double-column rectification combining the
condenser and evaporator to form a heat exchanger unit is still used today.

Condenser/reboiler The principle of double-column rectification is characterised by the

combination of condenser and evaporator to form a common heat exchanger unit. This
divides the rectification into two separate areas with different pressures

Any tray of the rectification column follows the same principle: The O₂ concentration of
the boiling O₂/N₂ liquid mixture F is greater than the O₂ concentration of the vapour D. A
certain volume of liquid corresponding to the same volume of reflux constantly flows from
the tray above into the liquid mixture below with an equivalent volume flowing down over
a weir onto the tray below. The vapour Du coming from the bottom tray penetrates the
liquid mixture F and has a higher O₂ content than the vapour mixture D. The O₂
concentration of the vapour Do rising from the upper tray is in turn less than that of the
vapour D. Thus a gas rich in nitrogen is obtained in the head of the column and a liquid rich
in oxygen is obtained in the sump of the column.

Structured packings

Significant progress in air separation technology was made in the mid-1980s. For the
first time, structured packings were used in cryogenic rectification. Packed columns work in
a similar way to sieve trays. The intensive contact between liquid and vapour required for
the rectification takes place on the huge surface area of the packing material. Liquid flowing
down becomes increasingly richer in oxygen, whereby the ascending vapour is enriched
with nitrogen. The main benefits of packed columns compared with sieve trays are a lower
pressure drop and consequently a lower power consumption for the air separation process.
Another important advantage of packed columns is the possible loading range including a
very high turn down to nearly 30%. This also forms the basis for a new process for argon
separation.
 What does a typical cryogenic air separation process look like?

1 Air compression → Compression of ambient air by a multi-stage turbo compressor

with intercoolers at a supply pressure of approx. 6 bar. → Removal of dust particles by a
mechanical air filter at the inlet of the compressor.

2 Air cooling and purification → Cooling of process air with water in a direct contact
cooler and removal of water soluble air impurities. → Chilling of cooling water in an
evaporation cooler against dry nitrogen waste gas from the rectification process. →
Removal of CO₂, water and hydrocarbons from the process air in periodically
loaded/regenerated molecular sieve adsorbers.

3 Cold production and internal product compression → Cooling of process air in heat
exchangers down to nearly liquefaction temperature by means of countercurrent with gas
streams from the rectification process. → Further compression of a sidestream of process
air by an air booster compressor. Expansion and cold production of the boosted air stream
in an expansion turbine. → Expansion and liquefaction of a sidestream of the boosted air in
a liquid separator. → Evaporation and warming to ambient temperature of the pumped
oxygen and nitrogen product in high-pressure heat exchangers.

4 Cryogenic rectification of air → Pre-separation of the cooled and liquefied air within
the pressure column into oxygen-enriched liquid in the column sump and pure nitrogen gas
at the column top. → Liquefaction of the pure nitrogen gas in the condenser/reboiler against
boiling oxygen in the sump of the low-pressure column. Liquefied nitrogen provides the
reflux for the pressure column and (after sub-cooling) for the low-pressure column. →
Different types of condenser are described in detail on page 16. → Further separation of the
oxygen-enriched liquid within the lowpressure column into pure oxygen in the sump and
nitrogen waste gas at the top.

5 Cryogenic rectification of argon → Argon-enriched gas from the low-pressure column

is transformed into oxygen-free crude argon by means of separation within the crude argon
column. → Pumping back liquid oxygen from the crude argon column sump into the low-
pressure column. Removal of the remaining nitrogen in the pure argon column.

What is rectification of air?

Rectification is synonymous with countercurrent distillation. This special distillation

separation process enables the individual components of a mixture to be separated with a
high purity combined with a good yield, even when their boiling points are relatively close
to each other. As a result of the different vapour pressures of the individual components
(pN₂ > pO₂), the composition of the vapour differs from that of the liquid mixture. The
vapour produced from a boiling liquid mixture of O₂/N₂ will thus have a higher N₂
concentration than the liquid mixture from which it originates.
 Air Separation Unit An ASU is used to separate the components of air and is used
extensively in industry today to produce high purity oxygen, nitrogen, and argon. Oxygen is
mainly used in metal production and chemicals and gasification. Gaseous nitrogen is used
in the chemical and petroleum industries and argon is primarily used for its inert properties
[12]. For high product demands, cryogenic distillation is preferred to adsorption methods
for separating air. Cryogenic distillation consists of compressing air and cooling it down to
cryogenic temperatures (around 100 K). Separation of the components is then carried out in
a staged vapor-liquid equilibrium unit (a cryogenic distillation column). A multi-stream
heat exchanger and an integrated reboiler/condenser are used for heat integration [13].
Cryogenic air separation is an energy intensive process and significant effort has been made
to reduce the electricity demand required for compression [10]. By as early as the 1970s, the
first computer aided attempts to design and control ASUs were made. Slight design and
operation changes to reduce energy consumption continue to be implemented to this day.
This has mainly been done by optimizing the heat and mass integration, implementing more
efficient machinery, and using advanced control strategies [12]. In cryogenic distillation,
the transition times for many of the control variables are on the order of hours. Adjustments
in the production level must consider the dynamics of the process to ensure that the
transitions are feasible. Several authors have studied the dynamic behavior and optimal
control of ASUs during production rate transitions.

Cryogenic pumps are used to circulate coolant in a variety of applications which also

include cooling high temperature superconducting cables or magnets, for cooling
synchrotron beamline crystals, and as pumps in prototype slush hydrogen applications.

To Maintain good performance of a cryopump;

Although our cryopumps are designed to provide high reliability and long-time continuous
operation, it is necessary to perform maintenance works on a regular basis.
It is important to perform daily checks to prevent failure.

Reciprocating cryogenic pumps have become key components within the industrial gas
industry handling primarily, liquid oxygen, argon and nitrogen. To ensure that pumps will
operate both safely and reliably it is important that pumps are correctly designed, installed,
operated and maintained as required for the duty. Pumping cryogenic fluids is accompanied
by some degree of hazard. The hazards include liquid under pressure, cryogenic
temperatures, volume and pressure increases due to vaporization and the ability of oxygen
to accelerate combustion. This document gives guidance to manage these hazards. This
publication has been prepared by member associations of the International Harmonization
Council, under the lead of EIGA and is intended for the worldwide use and application by
all members of the International Harmonization Council. The International Harmonisation
Council is composed of members from the Asia Industrial Gases Association (AIGA),
Compressed Gas Association, (CGA), European Industrial Gases Association, (EIGA), and
the Japanese Industrial and Medical Gases Association (JIMGA). Regional editions may
use non SI units and refer to national, and or regional legislation. Description of a
reciprocating cryogenic pump and pump installation and components A general
arrangement of a cryogenic pump installation consists of a vacuum insulated cryogenic
tank, reciprocating pump, a vaporizer, interconnecting and delivery pipework. A general
arrangement of cryogenic pump equipment is shown in Figure 1; not all required control
and safety elements are shown. Cryogenic pumping systems shall be designed to ensure that
required controls and safety elements are used in accordance with the application of the
system. Typical applications include filling of compressed gas cylinders, but there are other
applications where high pressure gas or cryogenic fluid is required.

Pump The reciprocating pump increases the pressure of the cryogenic fluid to the
required pressure of operation. Pump design has progressed and evolved over the years as
filling to higher cylinder pressures has increased. A variety of pump configurations are in
use. All have in common, provision for vapour escape, ideally back to the storage tank.
Modern designs enclose the cold end piston, barrel, suction and discharge valve assemblies
in a vacuum jacket. The pump is usually driven by an electric motor.

Suction filter To prevent damage to pumps, a filter should be fitted to the suction side
of the pump. Fine mesh filters (typically 150 microns or 100 mesh) are usually incorporated
within the pump suction chamber. Filters should have a large surface area and be readily
accessible for inspection or maintenance.

Cylinder assembly The main components are the piston, piston rings, cylinder and
suction and discharge valves. Piston rings are often made from a compound including
polytetrafluoroethylene (PTFE) or similar materials. Such plastics have a much larger
coefficient of expansion than that of the surrounding metals. Therefore it is important to
ensure that pumps are adequately cooled before operating, to reduce piston ring wear and
the risk of overheating.
 Gland seals Leakage of cryogenic liquid to the atmosphere from the piston assembly is
prevented by ‘low pressure’ gland seals around the piston rod. These can be damaged by
frozen moisture on the piston rod or excess play in the piston rod due to wear in the warm
end drive. Cryogenic liquid leakage through worn gland seals has resulted in brittle failures
of warm end drives and also oxygen related fires. Avoidance and detection of such leakage
is important, and may be accomplished by use of a thermal shutdown device such as a
thermocouple. An electrical seal heater or clamp on heater can be used on inert gases. If an
electrical seal heater or clamp is used for oxygen, the design shall limit the maximum heat
that can be put into the system or heater to prevent ignition conditions. The application of a
warm dry inert gas purge around the exposed piston rod can be used to extend the seal life.
NOTE The electrical seal heater should be in use during cold standby only. \

Warm end drive The piston is normally driven forwards and backwards by a crank
drive and crosshead assembly. These are usually of standard design, rated for the pressure
and flow rate expected for the cold end. Smaller, lower duty crank drives often have dry
running crossheads and pre-packed grease lubricated main rolling element bearings. Higher
duty crank drives are usually oil lubricated. NOTE For pumps in oxygen service the design
and selection of lubricants, materials, and purge gases is extremely important to safety.

Cold and warm end connection The warm and cold ends are often separated by a bolted
assembly that ensures both correct alignment and transmission of forces and that any
leakage of cryogenic liquid is kept away from the warm end. Correctly tightened bolts are
important to avoid fatigue related bolt failures. This is usually achieved by the use of a
torque wrench and appropriate lubricant on the washers, stud and nut threads.

Electric motors Electric motors can be single, dual or variable speed. The use of variable
speed drives gives additional flexibility for controlling filling rates and temperatures, for
example when filling small cylinders.

Air compressors work by forcing air into a container and pressurizing it. Then, the air is
forced through an opening in the tank, where pressure builds up. Think of it like an open
balloon: the compressed air can be used as energy as it's releasedAir compressors are
versatile and vital components of any factory or workshop. They’ve become smaller and
less bulky in recent years, making them more usable in various work situations. These are
highly useful portable machines that power single air tools.

The main advantage of air compressors is that they’re much more powerful than regular
tools, and they don’t require their own bulky motors. Since the only real maintenance that’s
required of them is a little bit of oiling, a variety of tools can be powered by a single engine
that utilizes air pressure for maximum potential.

Their versatility doesn’t just stop at the workbench for drills or sanders; they can be used
for anything from inflating a tire (like the ones at your local gas station) to unclogging the
sink at home.
 Air compressors are a testament to human ingenuity. It’s important to understand how
they work so you can choose the right air compressor for your project.
There are 3 styles of air compressor commonly found in mobile industrial
applications:

 Reciprocating, Piston Compressors.

 Rotary Screw Compressors.
 Rotary Vane Compressors
 How Each Type of Air Compressor Works
 There are two methods of achieving air compression: positive and dynamic
displacement. Each method has several sub-categories which we cover below. The
outcomes are relatively similar, but the processes to achieve them vary.
 Here’s how positive and dynamic displacement work:
 Positive Displacement

 Positive displacement air compressors force air in a chamber where the volume is
decreased to compress the air.

 Positive displacement is an umbrella term that describes different air compressors

that are power through positive air displacement. Although the internal systems vary among
different machines, the method of providing the power is the same.

 Some types of positive displacement compressors are better equipped for

industrial workloads while others are better for hobbyists or private projects. Here are the
three main types of air compressors that use positive displacement:

 1. Rotary Screw

 Rotary screw compressors have two internal “screws” that rotate in opposite

directions, trapping and compressing air between them. The two screws also generate
constant movement as they rotate around.

 This is a common type of air compressor and is one of the easiest to take care of.
The engines are typically industrial-sized and are great for continuous use.
  2. Rotary Vane

 Rotary screw compressors have two internal “screws” that rotate in opposite

directions, trapping and compressing air between them. The two screws also generate
constant movement as they rotate around.

 This is a common type of air compressor and is one of the easiest to take care of.
The engines are typically industrial-sized and are great for continuous use.

Reciprocating compressor.

A reciprocating compressor is a positive-displacement machine that uses a piston to

compress a gas and deliver it at high pressure. They are often some of the most
critical and expensive systems at a production facility, and deserve special attention.

Purpose and Applicability

Liquid nitrogen is one of the cryogenic liquids commonly used in research labs.  As
“cryogenic” means related to very low temperature, it is an extremely cold material.  It is
liquefied under high pressure condition and can expand to a very large volume of gas.  This
generic chemical safety guidance describes basic prudent safety practice for handling this
chemical in research labs. The principal investigator (PI) or the lab manager is responsible
for developing and implementing standard operating procedures (SOPs) for the purchase,
storage, and safe handling of this chemical that are specific to the PI’s research.

Hazards

Extreme Cold

The vapor of liquid nitrogen can rapidly freeze skin tissue and eye fluid, resulting in cold
burns, frostbite, and permanent eye damage even by brief exposure.

Asphyxiation

Liquid nitrogen expands 695 times in volume when it vaporizes and has no warning
properties such as odor or color.  Hence, if sufficient liquid nitrogen is vaporized so as to
reduce the oxygen percentage to below 19.5%, there is a risk of oxygen deficiency which
may cause unconsciousness. Death may result if oxygen deficiency is extreme.  To prevent
asphyxiation hazards, handlers have to make sure that the room is well ventilated when
using cryogens indoors.

Oxygen Enrichment

When transferring liquid nitrogen, oxygen in the air surrounding a cryogen containment
system can dissolve and create an oxygen-enriched environment as the system returns to
ambient temperatures. Since the boiling point of nitrogen is lower than oxygen’s, liquid
oxygen evaporates slower than nitrogen and may build up to levels which can increase the
flammability of materials such as clothing near the system. Equipment containing cryogenic
fluids must be kept clear of combustible materials in order to minimize the fire hazard
potential.  Condensed oxygen in a cold trap may combine with organic material in the trap
to create an explosive mixture.

Pressure Buildup and Explosions

Without adequate venting or pressure-relief devices on the containers, enormous

pressures can build upon cryogen evaporation. Users must make sure that cryogenic liquids
are never contained in a closed system. Use a pressure relief vessel or a venting lid to
protect against pressure build-up.

Handling

Prudent Safety Practices

 Liquid nitrogen should be handled in well-ventilated areas. 

 Handle the liquid slowly to minimize boiling and splashing. Use tongs to
withdraw objects immersed in a cryogenic liquid - Boiling and splashing always occur
when charging or filling a warm container with cryogenic liquid or when inserting objects
into these liquids. 
  Do not transport liquid nitrogen in wide-mouthed glass Dewars or Dewars not
protected with safety tape.
 Use only approved containers. Impact resistant containers that can withstand the
extremely low temperatures should be used.  Materials such as carbon steel, plastic and
rubber become brittle at these temperatures.  
 Only store liquid nitrogen in containers with loose fitting lids (Never seal liquid
nitrogen in a container).  A tightly sealed container will build up pressure as the liquid boils
and may explode after a short time. 
 Never touch non-insulated vessels containing cryogenic liquids. Flesh will stick to
extremely cold materials. Even nonmetallic materials are dangerous to touch at low
temperatures. 
 Never tamper or modify safety devices such as cylinder valve or regulator of the
tank 
 Liquid nitrogen should only be stored in well-ventilated areas (do not store in a
confined space). 
 Do not store liquid nitrogen for long periods in an uncovered container.   
 Cylinders and Dewars should not be filled to more than 80% of capacity, since
expansion of gases during warming may cause excessive pressure buildup.

Personal Protective Equipment

Eye/face protection 

A full face shield over safety glasses or chemical splash goggles are recommended
during transfer and handling of cryogenic liquids to minimize injuries associated with
splash or explosion. 

Skin protection

Loose-fitting thermal insulated or leather gloves, long sleeve shirts, and trousers without
cuffs should be worn while handling liquid nitrogen.  Safety shoes are also recommended
while handling containers.
 
A special note on insulated gloves: Gloves should be loose-fitting so they are able to be
quickly removed if cryogenic liquid is spilled on them. Insulated gloves are not made to
permit the hands to be put into a cryogenic liquid. They will only provide short-term
protection from accidental contact with the liquid.

Training

The PI is responsible for SOPs specific to use of this chemical in their lab. The PI/Lab
Manger is responsible for the site specific and hands-on training for the use of this chemical
in their lab. Training should be directly documented in the researcher’s lab notebook. On
each day of training, both trainer and trainee should sign the lab notebook. 

Initially, researchers should perform the procedures with the PI or senior researcher
present to observe the safe handling of this chemical. Review the reagent-specific safety
data sheets (SDSs). Evaluate the hazards associated with the chemical procedure and
experimental setup.

REPAIR AND MANTAINCE OF NITROGEN PLANT.

Leak Screening Techniques Leak screening in a DI&M program may include all
components in a comprehensive baseline survey, or may be focused only on the
components that are likely to develop significant leaks. Several leak screening techniques
can be used: Soap Bubble Screening is a fast, easy, and very low-cost leak screening
technique. Soap bubble screening involves spraying a soap solution on small, accessible
components such as threaded connections. Soaping is effective for locating loose fittings
and connections, which can be tightened on the spot to fix the leak, and for quickly
checking the tightness of a repair. Many methane emissions sources that are costeffective to
locate, measure, and fix are generally larger than the small leaks likely to be found by
soaping. However, because soap screening is rapid and of negligible cost, it can easily be
incorporated into routine maintenance procedures. Electronic Screening using small
handheld gas detectors or “sniffing” devices provides another fast and convenient way to
detect accessible leaks. Electronic gas detectors have catalytic sensors designed to detect
the presence of specific gases. Depending on the sensitivity of the instrument, detecting
leaks in areas with elevated ambient concentrations of hydrocarbon gas can be difficult.
Electronic gas detectors can be used on larger openings that cannot be screened by soaping.
Organic Vapor Analyzers (OVAs) and Toxic Vapor Analyzers (TVAs) are portable
hydrocarbon detectors that can also be used to quantify leaks. An OVA is a flame ionization
detector (FID), which measures the concentration of organic vapors over a range of 9 to
10,000 parts per million (ppm). A TVA is a combination device
 maintenance of a nitrogen plant
Containing both an FID and a photoionization detector (PID), which can measure
organic vapors at concentrations exceeding 10,000 ppm. Exhibit 1 shows a typical TVA,
consisting of a probe attached to a portable analytical instrument. TVAs and OVAs measure
the concentration of methane in the area around a leak. Screening is accomplished by
placing a probe inlet at an opening where leakage can occur. Concentration measurements
are observed as the probe is slowly moved along the interface or opening, until a maximum
concentration reading is obtained. The maximum concentration is recorded as the leak
screening value. Screening with TVAs is somewhat slow— approximately 40 components
per hour—and the instruments require frequent calibration. In larger facilities TVAs are
commonly used for volatile organic compound (VOC) leak screening, so these instruments
may be readily available to screen for methane leaks. Acoustic Leak Detection uses portable
acoustic screening devices designed to detect the acoustic signal that results when
pressurized gas escapes through an orifice. As gas moves from a highpressure to a low-
pressure environment across a leak opening, turbulent flow produces an acoustic signal,
which is detected by a handheld sensor or probe, and read as intensity increments on a
meter. Although acoustic detectors do not measure leak rates, they provide a relative
indication of leak size—a high intensity or “loud” signal corresponds to a greater leak rate.
Acoustic screening devices are designed to detect either high frequency or low frequency
signals. High Frequency Acoustic Detection is best applied in noisy environments where
the leaking components are accessible to a handheld sensor. As shown in Exhibit 2, the
acoustic sensor is placed directly on the equipment orifice to detect the signal. Acoustic
sensors are particularly useful for detecting leaking valves where the line vent is
inaccessible, such as blowdown valves and pressure relief devices connected to elevated
vent stacks Alternatively, Ultrasound Leak Detection is an acoustic screening method
thatdetects airborne ultrasonic signals in the frequency range of 20 kHz to 100 kHz.
Ultrasound detectors are equipped with a handheld acoustic probe that is aimed from a
distance at the potential leak source. Ultrasound detection is directional, making it possible
to pinpoint the location of leaks from distances as great as 100 feet. Although ultrasound
detection may be sensitive to background noise, this technique is useful for identifying gas
leaks at inaccessible equipment components. Infrared Cameras work according to the
principle that hydrocarbon emissions absorb infrared light in a certain wavelength.
Infrared (IR) cameras use this characteristic to detect the presence of gas emissions from
equipment by converting the scanned area into a moving image in real time such that the
gas plumes are visible due to their absorption of the IR light. Because of this, an IR camera
is able to screen hundreds of components per hour. An additional advantage is the ability to
screen inaccessible equipment: components in confined spaces or in elevated locations can
be screened remotely from an accessible location within viewing distance. In addition, IR
cameras can be hand-held for walking surveys of individual components, mounted on
trucks and other vehicles for close-range inspection over moderate distances, or mounted on
aircraft for aerial inspection to locate major leaks and vents over long distances. While it
may not be able to pinpoint individual leaking components with low leak rates, aerial
inspection is useful to screen many miles of transmissions pipelines or dispersed equipment
to detect plumes from large emissions sources. Leak Measurement Techniques An
important component of a DI&M program is measurement of the mass emissions rate or
leak volume of identified leaks, so that manpower and resources are allocated only to the
significant leaks that are cost-effective to repair. Four measurement techniques are
commonly used: Toxic Vapor Analyzers (TVAs) can be used to estimate mass leak rate.
Concentration measurements in ppm are converted to mass emissions estimates by means of
correlation equations. A major drawback to TVAs for methane leak measurement is that the
correlation equations are typically not site-specific. The mass leak rates predicted by
general TVA correlation equations have been shown to deviate from actual leak rates by as
much as three or four orders of magnitude. Similarly, a study conducted jointly by Natural
Gas STAR partners, EPA, the Gas Research Institute (GRI— now GTI, the Gas Technology
Institute), and the American Gas Association (AGA) found that measured concentration
thresholds, or “cut-off” values, such as 10,000 ppm or 100,000 ppm are ineffective for
determining which methane leaks are cost-effective to fix. Because the use of general TVA
correlation equations can increase measurement inaccuracy, the development and use of
site-specific correlations will be more effective in determining actual leak rates. Bagging
Techniques are commonly used to measure mass emissions from equipment leaks. The
leaking component or leak opening is enclosed in a “bag” or tent. An inert carrier gas such
as nitrogen is conveyed through the bag at a known flow rate. Once the carrier gas attains
equilibrium, a gas sample is collected from the bag and the methane concentration of the
sample is measured. The mass emissions rate is calculated from the measured methane
concentration of the bag sample and the flow rate of the carrier gas. Leak rate measurement
using bagging techniques is a fairly accurate (within ± 10 to 15 percent) but slow process
(only two or three samples per hour). Although bagging techniques are useful for direct
measurement of larger leaks, bagging may not be possible for equipment components that
are inaccessible, unusually shaped, or very large. High Volume Samplers capture all of
the emissions from a leaking component to accurately quantify leak emissions rates.
Exhibit 3 shows leak measurement using a high volume sampler. Leak emissions, plus a
large volume sample of the air around the leaking component, are pulled into the instrument
through a vacuum sampling hose. High volume samplers are equipped with dual
hydrocarbon detectors that measure the concentration of hydrocarbon gas in the captured
sample, as well as the ambient hydrocarbon gas concentration.