SUBMITTED TO:

Ms. Aliya Ahrar

SUBMITTED BY:
Waqas Mallick (CH-14078)
Arman Mallick (CH-14073)
Muhammad Usman Naseem
(CH-14057)
Muhammad Tauha Javed (CH-
14090)

COURSE CODE:
Process Modelling and

PRACTICAL Simulation (CH-401)

SUBMITTION DATE:
DISTILLATION February 1, 2018

API Operator Manual

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Table of Contents
Acknowledgement ............................................................................................................................................. 2
Introduction to API Operator Manuals ......................................................................................................... 3
How distillation works ...................................................................................................................................... 4
Unsteady State Distillation ........................................................................................................................... 4
Steady State Distillation ................................................................................................................................ 5
Multiple Still.................................................................................................................................................... 5
Distillation Column: ...................................................................................................................................... 7
Use of Fractionating Equipment ..................................................................................................................... 8
FOREIGN DEPOSIT AND TRAPS ....................................................................................................... 8
EXPLOSIVE MIXTURE ............................................................................................................................ 8
SHUTDOWN ................................................................................................................................................ 8
Normal Operations .......................................................................................................................................... 10
Operating variables and their relationships.............................................................................................. 10
Temperature ............................................................................................................................................. 10
Pressure ..................................................................................................................................................... 10
Flowrates ................................................................................................................................................... 10
BALANCES ON DISTILLATION COLUMN ................................................................................... 10
Material Balance .......................................................................................................................................10
Energy Balance.........................................................................................................................................10
QUALITY CHECK....................................................................................................................................11
Initial- End Boiling Point ....................................................................................................................... 11
Flash Point Test .......................................................................................................................................11
API Gravity .............................................................................................................................................. 12
Abnormal Operations .....................................................................................................................................13
Flooded Trays............................................................................................................................................... 13
High Levels ................................................................................................................................................... 14
Dry Trays ...................................................................................................................................................... 14
Trapped Water ............................................................................................................................................. 15
Upset Trays ................................................................................................................................................... 15
Conclusion ........................................................................................................................................................ 16
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Acknowledgement
We wish to express our sincere gratitude to our course teacher, Ms. Aliya Ahrar for providing us
the opportunity to go through this manual, understand the basics of the distillation in an easy way
and present it to the whole class. We also thank our fellow classmates for supporting us in this task.
We choose this moment to acknowledge their contributions gratefully. All our regards and respect
to all of them.
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Introduction to API Operator Manuals

As an operator of a refinery, a person must know the basics of all the processes and equipment
associated with it. The American Petroleum Institute (API) has therefore published a series of
manuals known as PILOT SERIES for the beginners who have just started or willing to be a worker
or operator in a refinery. Starting from the basics of chemistry and physics, these manuals provide
enough knowledge of the process and equipment that the person can understand the on-going
operation of a unit.
As far as designing and operations are concerned, these manuals only provide the most basic
knowledge of equipment and processes (like difference between continuous and batch distillation or,
at the highest level, which tray provides better vapor-liquid contact and what abnormal operations a
tower may face). There are no facts and figures related to the standards of designing of the
equipment as well as process variables. Consequently, an operator need not to have a detailed
knowledge about the process initially.

Figure 1: List of API Manuals

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How distillation works

The distillation is a separation technique used for centuries by the scientists and experts. This
technique was invented by a well-known Muslim scientist “Jabir Ibn-Hayyan”. As time went by,
the process was improved and certain changes were made to enhance the efficiency of the
technique. The continuous process was introduced and industries were applying more and more
variations in the processes to achieve separations in better ways. A brief explanation of the basic
classification is given below.

Unsteady State Distillation

Figure 2: Unsteady State Distillation

 Normally called batch distillation

 Feed enters the still, heat is provided and temperature is maintained until all the volatile
component is removed.
 Used for small-scale separations.
 High quality binary products
 Not suitable for refineries, large amount of product required
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Steady State Distillation

Figure 3: Steady State Distillation

 Efficiency of operation was greatly improved when unsteady state distillation was replaced
by steady state distillation, normally called continuous distillation
 Feed is introduced continuously in the still
 The liquid withdraws from the still is enriched in heavy liquid component
 Vapors are condensed in the condenser. The liquid collected at condenser is enriched in
pentane
 Vaporization is maintained in the still without change in temperature
Multiple Still

Figure 4: Multiple Stills with Multiple Heat Sources

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 PURITY of product is increased by using multiple still.

 The feed is introduced continuously in still 1
 Instead of being withdrawn completely from still 1 the liquid become the feed of still 2
 Boiling point of still3>still2>still1
 The vapors are condensed in the condensers in each still

Figure 5: Multiple Stills with Single Heat Source

 In this operation vapors are condensed only at still 1

 Heat is applied to still 3 only
 The vapors from still 3 are cycled back to still 2 and then cycled back to still 1
 The heat required to vaporize in still 1 and 2 are provided by recycled hot vapors
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Distillation Column:

Figure 6: Binary Distillation Column

 Stripping can be accomplished more efficiently in distillation column

 Each deck in the stripping section is equal to 1 still
 Because of the whole operation is carried out in one-unit, certain devices are necessary to
separate the devices from each other
 Distillation column consist of
 DECK: Each separation stage consists of a metal shelf called a plate or deck or tray
 RISERS: Vertical chimneys which let the vapors through the tray are risers
 BUBBLE CAP: Each riser is covered by a cap
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 DOWNCOMER: The passageway for a liquid down from one tray to the next is called
downcomer
WORKING:
 In the distillation column the feed enters near the top of the stripping section and passes
down through the downcomer on all trays in to the reboiler where heat is applied to the
mixture
 The hot vapors enter the lowest tray through the risers and bubble through the bubble cap
 As these vapors give up heat to the liquid some of the heavier vapor condense

Use of Fractionating Equipment

FOREIGN DEPOSIT AND TRAPS

 Blocked weepholes will hamper the the drainage of liquid from a tray during shutdown
 If liquid is unable to drain, a liquid trap will occur
 If water changes to ice, it cannot be drained from the tower
 The force of ice expanding against equipment may cause a metal to weaken or rupture

EXPLOSIVE MIXTURE

Every material has it different explosive ranges which can be seen by this chart

Normally, raising the pressure will widen the explosive range of hydrocarbon
Static electricity, heat, sparks, and iron can all be the source of ignition for an explosive mixture

SHUTDOWN

Before shutdown the tower, it is necessary to shutoff the heat of the tower
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If a vacuum occurs in a tower which is not designed for it, tower may collapse
To remedy this situation, a gas is taken itno the tower when it begins to cool
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Normal Operations

As a tower operator, you are responsible for producing products that meet specifications. If there is
a slight change in the specifications, the operator handles those problems by adjusting the concerned
parameters to retrieve the specifications and optimize the process.

Operating variables and their relationships

Temperature
Temperature has a significant effect on the composition of the product and varies under different
requirements, the variations illustrate the distribution of different temperature zones in different part
of the distillation column.
Product Temperature (High) Temperature (Low)
Top Too heavy (More) Light (More)
Bottom Too heavy (Less) Light (Less)
Side tray Heavy Light

Pressure
Under normal circumstances pressure is controlled automatically, though an operator always keeps
an eye on the readings and mostly remains unchanged until any abnormality occurs.

Flowrates
Flow rates are controlled by the operator according to the requirement of the product.

BALANCES ON DISTILLATION COLUMN

Material Balance

Column works on the principle of law of conservation of mass, what goes in must come out. The
whole column is in equilibrium and the column trays are also in equilibrium with each other.
Energy Balance

Like mass balance, energy also remain conserved in the distillation column, every tray is in
equilibrium (the rising vapours are in equilibrium with descending liquid droplets).
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QUALITY CHECK

Initial- End Boiling Point

Generally, a laboratory test to check the quality of the product, the sample is placed in a container
and heated, the vaporising from the sample pass through the condenser and are collected. The
temperature at which first droplet is collected is called initial boiling point the highest temperature
reached during the distillation column is called end boiling point. Graphical representation can be
shown by recording the temperature at the end of every 10 % collected. Commented [t1]:

Figure 7: Initial Point Tail and End Tail

 The liquid collected below 10% appears on graph as initial tail

 The liquid collected above 90% appears on the graph as the end.

 Distillation curve with long initial and end chain indicates the presence of both too much
heavy and light products.

Flash Point Test

Flash point is used to indicate the tendency of petroleum products to release flammable vapours.
The test is conducted by placing the cup of product and heating it slowly. at regular intervals the
vapours are exposed to the source of ignition. The point at vapours flashes is called flash point.
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API Gravity

API gravity is used to indicate the heaviness of petroleum materials and entirely opposite to the
specific gravity i.e. lighter the material higher the API gravity.
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Abnormal Operations
As an operator, the real challenges that need all the skills, a lot of knowledge and experience are the
abnormal operations in a tower. These situations are needed to be handled by a skillful operator who
knows all the causes and solutions to the situation.
An abnormal operation can have more than one cause and consequently, more than one solution. If
a problem arises, the operator applies the same orderly pattern of thought as in the normal
operations, the 4 C’s of problem solving. Furthermore, an operator must be skeptical about tests and
instruments. An abnormal situation may not be abnormal, just being shown because of any faulty
instrument.
In case of normal operations, usually temperature is adjusted to control quality of the products.
Abnormal tower presents many variables to deal with, and many alternatives for dealing with a single
problem. A skillful operator figures out the best possible way to correct the operation, keeping in
mind the safety of the personnel and the equipment. Cuz safety is numba one pioity!
Rate of deterioration is also an important factor in these conditions. The time until the problem gets
worse must be estimated before determining the solutions. Also, if one solution fails to make the
operation normal, there should be a second plan as a backup.
Following are some major abnormal situations that can arise in a tower.

Flooded Trays
 Resisting forces: Hydrostatic head (vapor), Pressure drop (liquid), Friction (both)
 Hydrostatic head in the downcomer vs hydrostatic head on the tray
 When depth of liquid in downcomer becomes greater than or equal to distance between two
plates, trays are flooded.
 Head increases due to increased pressure drop or amount of liquid
 Recognition:
1. Poor quality products
2. Little temperature gradient
3. Pressure drop larger than normal
4. Pressure fluctuates
 Possible Solutions: Reduce vapor or liquid flow.
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Figure 8: Tower flooded from tray 2 to 6

High Levels
 Constant height is maintained at the bottom
 Flooded tower and high liquid level tower behave same, except flooding can occur in any
part
 Observing difference in temperature from tray to tray, determine approximate location of
liquid level
 Possible solution: adjust the flowrate of bottom product

Dry Trays
 Results from overdraw of a product or from too hot vapor feed
 Overdrawing may remove all the liquid
 Tray provides no reflux below
 Trays below overdraw overheat
 Overheating produces heavier product above the drying section
 Too hot vapor enters as feed, vaporizes the liquid from the tray above
 Recognition: Poor quality, Little temperature gradient, Little pressure drop
 Possible solutions:
1. Decreasing the amount of product being drawn off
2. Reduce feed temp or increase reflux
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Trapped Water
 Tray filled with water, no longer effective
 Water remains trapped when temperature is below B.P. at that pressure
 Moisture in the feed
 Several trays become filled with water, they lose temperature gradient (T = B.P approx.)
 Removal:
1. Carefully and gradually increase temperature (for top). Water expands 1600 times
creating pressure surges.
2. Decrease temperature (for bottom)

Upset Trays
 Trays do not function properly
 By sudden high vapor velocities or by trapped water
 Trays are lifted, bubble caps may have torn loose
 Water remaining from turnaround or entering the tower during start-up
 Only fixed by hand
 Series of trays upset, little temperature gradient, smaller pressure drop
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Conclusion
This API Manual gave a brief but extremely useful information about the process of distillation and
has presented the essentials of fractionating process and the tower. By thoroughly going through this
manual, he will get to know the essentials of refining, the how and why of it, and he can use this
knowledge on the job.
The operator must go-through every manual in the PILOT SERIES to become an excellent and
skillful worker in his respective field. The more he knows, the more valuable he is to the company,
and the more satisfaction he finds in his job.