Operating & Maintenance Manual - SRU: Total, Lindsey Oil Refinery, Humberside, England

Comprimo Sulfur Solutions
Total,
Lindsey Oil Refinery,
Humberside, England
Operating & Maintenance

Manual - SRU
Project No.
64566-13
Project Name
Lindsey Oil Refinery
Document No.
64566-13/P.02/0011/A4
Revision
Prepared by
HELY
Checked by
BLGJ
Approved by
BLJ
Issue date : October 2006
Submitted by:
Jacobs Nederland B.V.
Plesmanlaan 100, 2332 CB Leiden
P.O. Box 141, 2300 AC Leiden
The Netherlands
Tel +31.71.582.7111 Fax +31.71.582.7050

A Subsidiary of Jacobs Engineering Group Inc.
Trade register: Rijnland 24301248
/var/www/apps/conversion/tmp/scratch_6/294995142.doc
Process Design Basis

Total Lindsey Oil Refinery
TABLE OF CONTENTS
1.0
INTRODUCTION
2.0
PROCES DESCRIPTION
2.1
2.1.1
2.1.2
2.1.3
2.2
2.2.1
2.2.2
2.2.3
2.2.4
2.2.5
2.3
DESCRIPTION OF THE APPLIED PROCESSES

CLAUS Process
Sulfur Degassing Process
Incinerator
DESCRIPTION OF PROCESS FLOW
Feed Gas System
Thermal Stage
Claus Catalytic Stages
Incinerator
UTILITY SYSTEMS
3.0
OPERATION AND CONTROL DESCRIPTION
3.1
3.1.1
3.2
3.2.1
3.2.2
3.2.3
3.2.4
3.2.5
3.3
3.3.1
3.3.2
3.3.3
3.3.4
3.3.5
3.4
3.4.1
3.4.2
TREATMENT OF CATALYST
Claus Catalyst Reactivation
NORMAL OPERATION
Operating Variables and Control
Plugging of Sulfur Locks
Ammonia Combustion
Draining K.O. Drums
Points for Consideration
PROCESS CONTROL, ALARM AND SAFEGUARDING SYSTEMS
Process Instrumentation
Instrument Alarm System
Safeguarding System
Controller, Alarm and Trip Settings
Relief Valves
TEMPERATURE RUNAWAYS
Fire inside the Claus Reactors
Fire in the Sulfur Pit
4.0
COMMISSIONING
4.1
4.1.1
4.1.2
4.2
4.2.1
4.2.2
INTRODUCTION
CLEANING OF WASTE HEAT BOILERS AND CONDENSERS
COMMISSIONING OF UTILITY AND INSTRUMENT SYSTEMS
NATURAL GAS INTAKE AND DRYING OUT
Introduction
Detailed Outline
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4.3
4.3.1
4.3.2
CATALYST LOADING
Stopping the unit
Catalyst loading
5.0
STARTUP
5.1
5.2
5.3
5.3.1
5.3.2
5.4
5.4.1
5.4.2
5.5
HEATING UP AFTER SHUTDOWN

CHECK LIST AND PREPARATION BEFORE FEED GAS INTAKE
FEED GAS INTAKE
Simplified Outline
Detailed Outline
STARTUP OF SULFUR DEGASSING SYSTEM
Initial Startup or Startup after a Long Shutdown
Startup after Short Interruption
TAKING IN SWS ACID FEED GAS
6.0
SHUTDOWN
6.1
6.2
6.2.1
6.2.2
6.3
6.3.1
6.3.2
6.4
6.4.1
6.4.2
6.4.3
GENERAL
SHUTDOWN PROCEDURE FOR SHORT PERIOD (HOT STANDBY)
Simplified Outline
Detailed Outline
SHUTDOWN PROCEDURE FOR LONG PERIOD (COMPLETE SHUTDOWN)
Simplified Outline
Detailed Outline
RESTART AFTER AN AUTOMATIC SHUTDOWN (TRIP)
Restart when the Unit is Hot and Sulfur is inside the Equipment
Restart when the Unit is Cold and Sulfur is inside the Equipment
Restart when no Sulfur is inside the Equipment
7.0
SAFETY
7.1
7.2
7.3
7.4
7.4.1
7.4.2
7.4.3
7.4.4
7.4.5
7.5
AMBIENT H2S MONITOR EQUIPMENT

SPECIAL SAFETY MEASURES AND INDUSTRIAL HYGIENE
FIRST AID MEASURES
TOXICOLOGICAL DATA
Physiological Effects of H2S
Physiological Effects of SO2
H2S Properties and Toxic Effects
SO2 Properties and Toxic Effects
Sulfur Dust
FIRE AND EXPLOSIVITY DATA
8.0
TROUBLE SHOOTING
8.1
8.2
8.2.1
8.2.2
INTRODUCTION
PROCESS PROBLEMS
General
Burner & Combustion Chambers
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8.2.3
8.2.4
8.2.5
8.2.6
8.2.7
8.2.8
8.2.9
8.3
8.3.1
8.3.2
8.3.3
8.3.4
8.3.5
8.3.6
8.4
Reactor Stages
Incinerator
Sulfur Degassing Vessel
Poor Sulfur Recovery
Pressure Drop
Plugging
Temperature Runaways
MECHANICAL PROBLEMS
Running Equipment
Ignitors
Boiler or Condenser Leakage
Refractory Material
Fluctuations and Hydrocarbon carry-over
Corrosion
CRITICAL AREAS IN SULFUR RECOVERY PLANT OPERATION
9.0
MAINTENANCE
9.1
9.1.1
9.1.2
9.1.3
9.1.4
9.1.5
9.1.6
9.1.7
9.1.8
9.1.9
9.1.10
9.1.11
9.1.12
9.1.13
9.1.14
9.1.15
9.1.16
9.1.17
9.1.18
EQUIPMENT
Knock-out Drums
Preheaters
Burners
Combustion Chambers
Waste Heat Boiler
Sulfur Condensers
Reactors
Sulfur Coalescer
Incinerator
Incinerator Waste Heat Boiler
Steam Superheater
Sulfur Locks
Sulfur Storage Tank
Steam Coil in Sulfur Degassing Vessel
Running Equipment
Piping and Valves
Analyzers
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1.0
INTRODUCTION
The Sulfur Recovery Unit is designed to recover sulfur from sour gases originating
from the following sources:
The Amine Regeneration Unit

The Sour Water Stripper Unit
The process design is based on the CLAUS process to recover elementary sulfur
from an H2S containing gas stream.
The SRU consists of a thermal stage, in which H2S is partially burnt with air, followed
by three catalytic Claus stages. The tail gas from the final stage is routed to the
incinerator.
Facilities are provided for continuous degasification of the produced sulfur to reduce
its H2S content.
The instructions contained herein are presented as a general guide to aid in safe
startup and operation of the unit.
Operating experience will indicate where a procedure should be modified to improve
the performance of the unit.
These instructions are to be used in combination with:
Process Flow Scheme.
Piping and Instrument Diagram.
Description of Logic System for Startup and Shutdown Operation.
Cause & Effect Diagram for Normal Operation.
Basis of design.
Process control narrative(s).
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2.0
PROCES DESCRIPTION
2.1
DESCRIPTION OF THE APPLIED PROCESSES
2.1.1
Claus Process
Thermal reaction stage
In the applied sulphur recovery process, known as conventional Claus process, 'air to - acid gas ratio' is maintained to produce an H2S - to - SO2 ratio of exactly 2/1 in
the catalytic effluent gases. This is the optimum ratio of H2S - to - SO2 for the Claus
reaction.
The main reaction in the main burner and reaction furnace is:
3
H 2S + O 2 SO 2 + H 2 O + heat
2
The major percentage of the residual H2S combines with the SO2 to form sulphur,
according to equilibrium reaction:
3
2H2 S + SO 2
S 2 + 2H2 O - heat
2
By this reaction, known as the Claus reaction, sulphur is formed in vapour phase in
the main burner and reaction furnace.
Catalytic Claus stage
The downstream catalytic reaction stage further increases the overall conversion to
sulphur. In the first, second and third reactor the following reaction takes place:
2 H2S + SO2 3/x Sx + 2 H2O + heat
The Claus equilibrium is shifted to the sulphur side by making use of a Claus
catalyst. Condensation and removal of sulphur after the first, second, and third
reactor enables further conversion of sulphur in the next catalytic stage.
2.1.2

The sulphur produced in the SRU contains about 300 ppm wt H2S, partly chemically
bound as polysulphides (H2Sx) and partly physically dissolved. To remove H2S and
H2Sx from liquid sulphur, eliminating potential toxic and explosion hazard associated
with handling, transport and storage of liquid sulphur, the Shell Sulphur Degassing
Process has been developed. Degasification by means of the Shell degassing
process reduces the H2S content to less than 10 ppm wt.
Degasification is obtained by injecting air via spargers in the liquid sulphur, thereby
partly stripping the dissolved H2S from the sulphur and partly oxidizing it to
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elemental sulphur. Furthermore, the removal of H2S from the sulphur promotes the
decomposition of the polysulphides into H2S and sulphur.
H2Sx H2S + Sx-1
H2S + O2 1/x Sx + H2O
2.1.3
Incinerator
The tail gas resulting from the Claus stage and vent gas from the sulphur degassing
still contains traces of sulphur compounds. These sulphur compounds are oxidized
in the incinerator at elevated temperatures. The main reactions are:
H2S + 3/2 O2 SO2 + H2O
1/x Sx + O2 SO2
COS + 3/2 O2 SO2 + CO2
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2.2
2.2.1
DESCRIPTION OF PROCESS FLOW

Feed Gas System
Feed gas to the SRU consists of the following different streams:
Acid gas from HDS-1 unit
Acid gas from HDS-3 unit
Part of acid gas from HDS-2 unit
Sour gas (H2S and Ammonia) from SWU-8 unit
There is an acid gas interconnection line that provides the refinery with the option to
redistribute the feed streams in the event of an outage on one of the SRU units.
The acid gas from the HDS units and sour H2S gas from the SWU-8 combine
upstream of the acid gas knock-out drum 13D-01. The Ammonia gas stream from
the SWU-8 unit is routed to a dedicated sour gas knock-out drum 13D-02. The
Ammonia stream will normally be routed direct to the Incinerator 13F-04. However
there is an option to destruct the Ammonia by combining with the acid gas down
stream of the knock out drums. The combined feed gas is routed to the Main Burner
13F-01. In the Knock-out Drums the entrained water is separated from the feed
gases. The sour water is intermittently drained to the Amine drain tank on the ARU.
2.2.2
Thermal Stage
Main Air Blower 13B-01A/B supplies the air to the main burner. The main air blower
also supplies air to the sulphur degassing system. The combustion temperature in
the combustion chamber has to be sufficiently high (above 1250C) for NH3
destruction in the reaction furnace. The air to the main burner is exactly sufficient to
accomplish the complete oxidation of all hydrocarbons and ammonia present in the
feed gases and to burn H2S.
The combustion air to the main burner is controlled by the Advanced Burner Control
system (ABC system). This system is based on the feed forward control. Reference
is made to the control description, doc. no. 64566-13/P.02/0007/P.
The required quantity of air is calculated by measuring the acid feed gas flow, the
SWS Ammonia gas flow and natural gas flow and multiplying each flow with its own
individual air demand (feed forward control). This results in a total air demand and
this signal sets the flow control system in the air supply. The flow control system
adjusts the position of two control valves.
The system adjusts immediately a small control valve in the trim air line, after which
the bigger main valve follows with a delay. The final situation is that the flow through
the control valve in the trim air line is again in the optimum of its range to cope
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quickly with flow changes. Then the total air flow through the main air and the trim
air lines corresponds with the total amount of acid gas feed.
The combustion temperature has to be sufficiently high (1250C minimum) to obtain
a proper destruction of NH3. The feed gas does not contain sufficient combustibles
to obtain this temperature. Therefore preheating of the acid gas using jacketed
piping is required. When even with preheating this temperature is not met, Natural
gas has to be co-fired in the main burner. The Natural gas is used instead of
Refinery Fuel Gas as it has a more stable in composition, to enable better ratio
control of the air to fuel ratio. Excess sub or over stoichiometric combustion may
lead to damage of the catalyst.
The supply of Oxygen will be via a dedicated gun to the main burner. This will only
be used when operating away from the base design case where an increased
throughput or Ammonia destruct options are required.
To remove the heat generated in the main burner 13F-01, the gas passes through
the tube bundle located in Waste Heat Boiler 13E-01. The gas is cooled, thereby
generating saturated high pressure steam, which is collected in Waste Heat Boiler
Steam Drum which is a part of the waste heat boiler. The WHB high pressure steam
combines with the steam generated from the Incinerator WHB (13E-11). The
combined saturated HP steam is routed through a Steam Dryer (13D-11), before
partly supplying the Re-heaters (13E-03/05/07). Any excess being superheated (in
the Incinerator 13E-12) and exported into the HP steam header. Boiler feed water
is introduced to the steam drum of the waste heat boiler on level control.
The process gas is cooled further in the First Sulphur Condenser 13E-02. The
sulphur vapour in the process gas is condensed and separated from the gas. Liquid
sulphur from the first sulphur condenser is directed to the Sulfur degassing vessel
13D-08 via its Sulphur lock 13D-06A. A demister pad is installed in the outlet
channel of the first sulphur condenser to recover liquid sulphur, entrained as mist
with the process gas.
In the sulphur condenser low pressure steam is generated.
2.2.3
Claus Catalytic Stages

The gas stream from the first sulphur condenser is heated again in the First
Reheater 13E-03, to obtain the optimum temperature for the catalytic conversion in
the First Claus Reactor 13D-03. The first Claus reactor contains a top layer of
alumina oxide type catalyst and a bottom layer of titanium oxide catalyst to obtain a
high COS and CS2 conversion in the bottom the bed. The steam flow to the first
reheater is adjusted by a temperature controller at the inlet of the reactor.
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In the reactor, the H2S and SO2 in the process gas react over the catalyst until
equilibrium is reached. The inlet temperature of the reactor is maintained at 240C
to favour COS and CS2 conversion. The process gas from the reactor passes into
the Second Sulphur Condenser 13E-04, is cooled and the sulphur in the gas is
condensed and separated from the gas. Liquid sulphur from the second sulphur
condenser is directed to the Sulphur degassing vessel via its Sulphur lock 13D-06B.
A demister pad is installed in the outlet channel of the second sulphur condenser to
recover liquid sulphur, entrained as mist with the process gas. Like in the first
sulphur condenser low pressure steam is generated.
The gas stream from the second sulphur condenser is heated again in the Second
Reheater 13E-05, to obtain the optimum temperature (210C) for the catalytic
conversion in the Second Claus Reactor 13D-04 which contains an alumina oxide
type catalyst. The steam flow to the second reheater is adjusted by a temperature
controller at the inlet of the reactor. The inlet temperature is lower than in the first
reactor to promote a high conversion of H2S and SO2 into sulphur.
In the reactor, the H2S and SO2 in the process gas react over the catalyst until
equilibrium is reached. The process gas from the reactor passes into the Third
Sulphur Condenser 13E-06, is cooled and the sulphur in the gas is condensed and
separated from the gas. Liquid sulphur from the third sulphur condenser is directed
to the Sulphur degassing vessel via its Sulphur lock 13D-06C. A demister pad is
installed in the outlet channel of the third sulphur condenser to recover liquid
sulphur, entrained as mist with the process gas.
The first, second and third sulphur condensers are combined in one shell. Boiler
feed water is introduced to the shell side of the condensers on level control. The
condensers generate low pressure steam which is used for plant heating, the
surplus is exported to the refinery steam network.
The gas stream from the third sulphur condenser is heated again in the Third
Reheater 13E-07, to obtain the optimum temperature (195C) for the catalytic
conversion in the Third Claus Reactor 13D-05. This reactor contains alumina oxide
type catalyst. The steam flow to the third reheater is adjusted by a temperature
controller at the inlet of the reactor; the inlet temperature is lower than in the first two
reactors to promote a high conversion of H2S and SO2 into sulphur.
The process gas from the third Claus reactor passes to the fourth Sulphur
condenser 13E-08, is cooled and sulphur in the gas is condensed and separated
from the gas. Liquid sulphur is directed to the Sulphur degassing vessel via its
Sulphur lock 13D-06D. A demister pad is installed in the outlet channel of the fourth
sulphur condenser to recover liquid sulphur, entrained as mist with the process gas.
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Boiler feed water is introduced to the shell side of the fourth condenser on level
control. The 4th condenser generates a small amount low pressure steam that is not
used for plant heating and is condensed back using the LLP Steam condenser 13E09. Part of this condensate is used in the sulphur cooler 13E-10, part of the
Degassing Vessel 13D-08, and returned into the closed system as LLP steam
upstream of the air cooler 13E-09.
The process gas flows from the fourth sulphur condenser into the downstream
Coalescer 13D-07, provided with a demister pad, in which the last traces of liquid
sulphur are separated from the gas and the liquid sulphur is sent to Sulphur
degassing vessel via its Sulphur lock 13D-06E.
2.2.4
Incinerator
The Claus tail gas and the vent gas from the sulphur degassing vessel contain
residual H2S and other sulphur compounds, which cannot be released directly to the
atmosphere. These gases are therefore thermally incinerated in incinerator to
convert residual H2S and sulphur compounds into SO2. The Ammonia stream from
the SWS will normally be fed direct to the Incinerator from the Sour Gas Knock Out
Drum 13D-02. There is an option to feed to thermal section for Ammonia
destruction, but this will not be the normal operating case. Additionally the vent
gases from the SWS buffer tanks are also fed to the incinerator.
The gases to be oxidised are heated by mixing with hot flue gas, obtained by
combustion of fuel gas in Incinerator burner 13F-02.
The fuel gas flow to the burner is adjusted by control of the temperature in the flue
gas leaving the incinerator. The combustion air for the fuel gas is provided by the
Incinerator blower 13B-02. Main air blower 13B-01B can also be used as a spare
for the incinerator blower using the pressure letdown control valve PCV010
The air supply to the incinerator is divided in three stages:
1. Primary air used for substoichiometric combustion of fuel gas
2. Staged air for supply of air to the flue gas from the burner to obtain
overstoichiometric combustion of the fuel gas.
3. Secondary air for combustion (oxidation) of the process gas
The primary air flow is ratio controlled by the fuel gas flow. The resulting primary air
flow rate is 80% of the amount required for stoichiometric combustion of the fuel
gas. This reduces the formation of NOx in the burner.
The staged air flow is also ratio controlled by the fuel gas and amounts to 30% of
the air flow rate required for stoichiometric combustion of the fuel gas.
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An oxygen analyser is situated in the oxidiser flue gas and is provided with an
oxygen controller. The signal from the oxygen controller is the setpoint of the flow
controller of the secondary air. The staged air flow and secondary air flow rates are
therefore adequate to supply sufficient oxygen to burn the un-burnt fuel gas and to
incinerate the combustibles in the process gas. It results in an oxygen excess of
2.1 vol.% in the incinerator flue gas. The oxygen excess ensures that the flue gas
contains less than 10 ppm vol. H2S.
The flue gas leaving the incinerator is cooled to about 500 C in the Steam
Superheater 13E-12, prior to entering the incinerator waste heat boiler 13E-11. Here
the flue gas is further cooled (to 300oC), thereby producing saturated HP steam.
This is combined with the main WHB (13E-01) steam as described above.
2.2.5

The liquid sulphur from the condensers is first cooled in the Sulphur Cooler 13E-10
which is installed in the sulphur degassing vessel 13D-08.
The sulphur as it is produced in the sulphur recovery train contains about 300 ppm
wt H2S. Sulphur stripping has been incorporated to reduce the H2S content to less
than 10 ppm wt. It takes place in the stripping section of the degassing vessel.
Two bubble columns are located in the stripping section. They are identical and
have a rectangular cross section. The top and bottom parts are open. Air distribution
spargers are provided at their bottom sides.
The stripping air to the spargers is supplied by the main air blower (13B-01A/B). The
function of the air is to obtain forced sulphur circulation in and around the bubble
columns, to strip the dissolved hydrogen sulphide from the liquid sulphur and to
oxidize the major part of the H2S to sulphur. Furthermore, the removal of H2S from
the sulphur promotes the decomposition of polysulphides into dissolved H2S and
sulphur. In this way, sulphur with a H2S content of less than 10 ppm wt is obtained.
Besides the stripping air, an additional amount of sweep air is added via the air
inlets, located on the cover of the degassing vessel. The sweep air is also supplied
by the main blower (13B-01A/B). The total air, together with the H2S released from
the sulphur, is taken to incinerator 13F-04.
The degassed sulphur is pumped by the Sulphur Pump 13P-01A/B from the vessel
to sulphur storage tank 13D-12. The Sulphur pump is automatically stopped when
the level drops too much. One installed stand by pump is provided in the degassing
vessel. Vessel and pump sumps are equipped with steam coils to maintain the
temperature of the sulphur.
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The storage tank can contain 10 days sulphur production. Sulphur from storage tank
is pumped by the Sulphur transfer Pump 13P-02 to the solidification unit.
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2.3
UTILITY SYSTEMS
High Pressure (HS) Steam
Saturated HS steam is generated in both waste heat boilers (13E-01/11). It is
utilized as heating medium for the steam Reheaters (13E-03/05/07). Surplus HS
steam is superheated via a coil between the Incinerator (13F-04) and Incinerator
WHB (13E-11), and is routed to the HS steam system.
During start-up and shutdown when the waste heat boiler produces insufficient HS
steam it might be necessary to import HS steam from the refinery system to supply
steam to the reheaters.
Low Pressure (LS) Steam
Saturated LS steam is generated in the first three sulphur condensers (13E02/04/06) and used for plant heating (e.g. for degassing, tracing/jacketing of
pipelines). The remainder is discharged into the LS steam system. An MP steam
import line is in place to support in the internal LP header in the event of drop in
pressure.
During hot standby LS steam is supplied to the main burner for cooling of the fuel
gas flame, as air cooling is not allowed under these circumstances.
Discontinuous steam purges may be required as smothering medium during a
temperature run-away in the sulphur vessel.
When the equipment in the unit is cold (below 100C), steam should not be
introduced into the main burner, neither for cooling nor for purging.
Boiler feed water
Boiler feed water is supplied to the waste heat boilers and the sulphur condensers.
Fuel gas
Fuel gas is fired in the incinerator burner. During startup, hot standby and shutdown
or in the case that the flame temperature is lower then 1250C.
Nitrogen
A continuous small nitrogen purge is required for the flame scanners, sight glasses
and pyrometer of the main burner and the relief line of the SWS gas knock out drum.
During startup it is also used for purging the main burner and the reaction furnace.
Condensate recovery
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All the steam used for heating within the plant shall be recovered. Each item is first
routed to a steam trap, to take care of the correct conditions within the item where
the heating takes place.
The condensates from the LS steam used for internal heating are routed to the
condensate return header. The steam generated on the 4th condenser 13E-08 is
condensed by the LLP Steam condenser 13E-09 and drained back to the flash
drum. A small part of this condensate is used in the sulphur cooler 13E-10, with the
LLP steam generated returned upstream of the LLP Steam condenser 13E-09.
Blow down recovery
The blow down of both waste heat boilers and the sulphur condensers are routed to
the Blow down Drum 13D-10, where it is completely flashed to atmospheric
pressure. The blow down water is quenched with Raw water to approx. 60C before
being routed to the sewer.
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3.0
OPERATION AND CONTROL DESCRIPTION
3.1
TREATMENT OF CATALYST
3.1.1
Claus Catalyst Reactivation

Sulfate reduction (rejuvenation)
The main cause of aging of alumina type catalyst is the formation of "superficial
sulfate" by the reaction of sulfur dioxide (present in the process gas) with the
alumina of the catalyst whether in the presence of oxygen or not.
This interaction between sulfur dioxide, oxygen and alumina is greater at higher
temperature and partial pressure of oxygen. Reversibly a reduction by hydrogen
sulfide or by a mixture of H2S and SO2 starts at 250 - 300C.
A decrease of sulfur recovery is often caused by deactivation of the catalyst due to
sulfation. Sulfates are mainly formed by excess oxygen during shut-down operation.
Therefore, immediately after restart, the catalyst should be reactivated. Also, if
required, the catalyst can be reactivated during operation. Reactivation (also called
regeneration or rejuvenation) is the reduction of sulfates at elevated temperature (as
high as possible) with slight excess of H2S (2 3 vol.%). The rejuvenation procedure
is only applicable for the 2nd Claus reactor. The titanium catalyst (CSR_31) which is
installed in the 1st Claus reactor is insensitive to sulfation and does not require
rejuvenation.
The velocity of this reduction reaction is fairly high in the range of 250 - 300C
compared to the velocity of the sulfation reaction.
When contacted with H2S the superficial sulfate reacts to sulfur and water.
As long as the surface area of the catalyst is above 150 m2/g and the activity
decrease is the result of an incidental sulfation, an improvement can be expected by
operating the second reactor as follows:
Increase the H2S content in the gas to the reactor to 2 - 3 vol.%

Increase the reactor inlet temperature to the maximum possible.
Maintain these conditions for at least 24 hours.
An increase of the H2S content in the gas to the second reactor is obtained by
operating the main burner with a deficiency of air. Therefore, an adjustment of the
ratio air-to-feed gas or set point of the H2S analyzer controller has to be made.
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In order to reach the maximum temperature in the reactor, the steam supply to the
reheater is fully open and the plant throughput is decreased to approximately 50% of
the design feed.
Catalyst reactivation is advised after each shutdown operation.
The first reactor contains a titanium-based catalyst, which is insensitive for sulfation,
with a top layer of alumina type catalyst. The top layer protects the titanium catalyst
against soot deposition. Because of the elevated temperature in the first reactor and
the high H2S content, sulfation of the top layer will hardly occur.
Sulfur removal (heat soak)
During operation, sulfur is absorbed inside the pores of the catalyst. This has no
adverse effect on the performance of the plant. When, however, during operation the
bed temperature is lower than the sulfur dewpoint, sulfur condenses on the surface
of the catalyst, which reduces the catalyst activity. This applies only for the catalyst
in the 2nd and 3rd reactor as the 1st reactor operates always far above the sulfur
dewpoint.
The dewpoints of the gas leaving the 1st, 2nd and 3rd reactors are 247C, 216C and
182C, respectively.
As soon as a decline in temperature difference over a reactor becomes noticeable
from the daily operating figures, the most likely reason is that too much sulfur has
accumulated on the catalyst. To remove the sulfur from the concerned catalyst bed,
the reactor inlet temperature should be increased approximately 20 C for a period
of at least 24 hours. Reduce plant capacity if required to obtain this temperature
increase. It should be noted that this operation does not reverse the aging of Claus
catalyst.
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3.2
NORMAL OPERATION
3.2.1
Operating Variables and Control

Main burner
For a detailed description and explanation of the combustion air control system
(ABC system), reference is made to the "Process Control Narrative for the
Advanced Burner Control System (ABC)", document no. 20507-6456613/P.02/0007.
For an optimum performance of the plant it is required that the correct amount of air
is added in the burner to the acid feed gas. This amount of air is the air required for
combustion of slightly less than 1/3 of the total H2S present in the feed gas and the
air required for the other combustibles in the feed gas (hydrocarbons and ammonia).
The H2S concentration in the tail gas from the fourth sulfur condenser is measured
by an analyzer (AT-111) and subsequently controlled by AC-111, so that control at
(H2S - 2SO2) = zero is obtained. This corresponds with (H2S : SO2) = 2. Then the
highest possible sulfur recovery rate is obtained.
In the hot standby mode only natural gas is burned in the main burner. The
combustion is slightly substoichiometrical to avoid oxygen break-through to the
reactor stages. Without cooling the flame temperature would be too high. Therefore,
steam as a cooling medium is injected into the flame. The steam flow rate is
approximately four times the natural gas flow rate on weight basis.
Flame temperature
It is imperative that the combustion temperature in the main burner is at least
1250C to destroy the NH3 present in the Sour Water Stripper acid gas. When the
feed gas contains not sufficient combustibles to maintain the required flame
temperature, additional heat is supplied. This is obtained by preheating both the air
and the amine gas feed. The feed gas preheater will also be maintained in operation
when no SWS feed gas is supplied to avoid water condensation in the acid gas feed
line. If necessary it is advised to increase the flame temperature of the main burner
above 1250C by co-firing natural gas.
Claus reactor stages
When the reactor inlet temperatures are according to the design values the
conversion to sulfur is maximum. At a lower inlet temperature of the first reactor,
consequently the outlet temperature is also lower. A temperature lower than 300C
leads to insufficient conversion of SOC and CS2. This is not recovered in the
downstream part of the unit and results in an increased SO2 emission from the
stack.
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At a lower inlet temperature of the second reactor, sulfur vapor may condense on
the catalyst bed, resulting in reduced catalyst activity. At higher temperatures, less
H2S is converted as the equilibrium shifts to H2S and SO2.
At high throughput, the reactor inlet temperatures are 240C and 205C,
respectively. When the unit operates at low throughput (below 40% of design), it is
advised to increase the inlet temperature of the second reactor by 10-15C, to
compensate for heat losses to obtain a safe dew point margin. This prevents sulfur
condensation on the catalyst bed. The reactor inlet temperatures are automatically
controlled: the controllers adjust control valves in the steam supply lines to the
reheaters.
The difference between the inlet and bottom temperature of the reactor is a measure
for the conversion rate in the catalyst bed. As soon as a decline in temperature
difference across the second reactor becomes noticeable from the daily operating
figures, the inlet temperature should be temporarily increased. In this way
condensed sulfur evaporated from the catalyst bed. It is pointed out that
condensation of sulfur on the catalyst is the most likely reason for deterioration of
the catalyst.
Figure 1: Relative SO2 formation
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First, second and third sulfur condenser

The condensers are operated at a convenient steam pressure to be able to enter the
refinery low pressure steam system. The set point of the pressure controller is kept
above the refinery pressure in order to overcome the pressure losses inside the
sulfur plant at the one hand to stabilize the steam pressure in order to maintain
constant sulfur condenser outlet temperatures at the other hand.
Fourth sulfur condenser
The steam pressure in the condenser is low in order to condense as much sulfur
vapor as possible, but not so low that the water temperature causes solidification of
sulfur (approx. 116C).
During the first days after admitting Claus tail gas to the fourth stage, the condenser
is operated at an increased steam pressure (approx. 3 barg.) to avoid plugging of
the condenser by solidification of sulfur. This may also be done at low throughput
operation.
In case of air fin cooler failure, the steam pressure rises until the set pressure of the
pressure relief is reached. Then the steam is blown off to atmosphere. Under these
conditions, boiler feed water shall be supplied to maintain the water level. It is better
to use the vent to control the steam flow/ pressure.
Incinerator
For a description and explanation of the incinerator control system, reference is
made to the process control narrative, doc.nr. 20507-64566-13/P.02/0008. The
function of the incinerator is to convert the residual H2S and other sulfur compounds,
present in the off-gas and the vent gas from the sulfur pit, into SO2. The maximum
allowable H2S content in the flue gas from the incinerator is 10 ppm vol.
The gas to be oxidized is heated by mixing with hot flue gas. The hot flue gas is
produced in the incinerator burner by combustion of fuel gas with air. The
combustion air for the natural gas is supplied by the incinerator air blower. The air
required for oxidizing the sulfur compounds is partly supplied as vent air from the
sulfur pit at a constant quantity. The remainder is supplied by the incinerator air
blower. The natural gas is burnt in two stages.
The first stage is the primary air, supplied to the burner. The primary air flow is ratio
controlled by the natural gas flow. It is important to operate the primary air at
substoichiometric conditions (between 80% and 90% of stoichiometry) to prevent
NOx formation.
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The next stage is the "staged" air, supplied after the flame zone. The staged air flow
is also ratio controlled by the natural gas flow, but moreover the output of the oxygen
controller is added to the air flow rate, calculated from the natural gas flow.
Consequently, free oxygen is available for the incineration of non-recovered sulfur
components. The oxygen-analyser is controlled at an oxygen content of 1.7% by
volume.
The flue gas leaving the incinerator is discharged via the stack to the atmosphere.
The operating temperature in the incinerator is 760C. It is obtained from:
1. Combustion of fuel gas in the incinerator burner.
2. Combustion of the combustibles present in the tail gas.
At lower temperatures than 725C the H2S content in the flue gas will increase. This
might be partly compensated by increasing the O2 concentration. A higher
temperature will result in higher fuel gas consumption. In the Claus mode, the tail
gas contains considerably more H2S. In order to keep the H2S content in the flue gas
below 10 ppm vol., the operating temperature should be increased.
A low O2 concentration has the same effect as a low temperature: the H2S content
increases. More O2 means that too much air is supplied, resulting in high fuel gas
consumption.
The flue gas leaving the incinerator is discharged via the stack to the atmosphere.
Apart from at initial startup, the incinerator should be started before the main burner
at subsequent startups. Then poisonous gas that might still be present in the
equipment, is converted and released via the stack.
Steam Superheater
The steam superheater should always have steam flowing through the tubes when
the incinerator is in operation. The steam flow prevents overheating of the tubes.
During startup, when no steam is jet produced by the waste heat boiler in the unit,
steam has to be imported from the refinery. When the Waste heat boiler produces
enough steam, the steam import from the refinery system can be stopped.
Sulfur degasser
Liquid sulphur coming from the condensers is cooled in the sulphur cooler before
entering the degassing vessel. This liquid sulfur contains about 300 ppm wt H2S. To
reduce this to less than 10 ppm wt, the sulfur is stripped in the degassing vessel.
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Two bubble columns are located in the stripping section. Air distribution spargers are
provided at their bottom sides.
The stripping air to the spargers is supplied by the main air blower (13B-01A/B). The
function of the air is to obtain forced sulphur circulation in and around the bubble
columns, to strip the dissolved hydrogen sulphide from the liquid sulphur and to
oxidize the major part of the H2S to sulphur. Furthermore, the removal of H2S from
the sulphur promotes the decomposition of polysulphides into dissolved H2S and
sulphur. In this way, sulphur with a H2S content of less than 10 ppm wt is obtained.
3.2.2
Plugging of Sulfur Locks

Plugging of sulfur locks or sulfur rundown lines can be detected by checking the
funnels. Please note that personnel protection should be used, see also section 7.2.
The system is plugged when no liquid sulfur flows. When a sulfur lock is plugged, an
LP steam or nitrogen hose can be connected to the top of the lock. The block valve
in the sulfur rundown line is closed and the lock is blown with the steam or nitrogen.
If plugging occurs in the sulfur rundown line, the sulfur lock outlet is to be blindedoff. Then lock and sulfur lines are blown in the direction reverse to normal flow.
Especially the sulfur locks downstream the fourth condenser and the coalescer shall
be checked regularly at least on a daily basis. Because of the relatively low
temperature, the danger of plugging is here higher.
3.2.3
Ammonia Combustion
The feed gas from the Sour Water Stripping Unit contains ammonia. It is imperative
that the ammonia is converted in the combustion chamber as completely as possible
so that the process gas through the equipment contains only a few ppms of
ammonia. Incomplete conversion of ammonia will cause plugging by ammonium
salts on the coldest spots in the equipment (condenser outlets)
Good ammonia conversion is ensured when the temperature of combustion in the
main burner and combustion chamber is sufficiently high and the residence time is
long enough. Especially the combustion temperature should be at least 1250C
during the whole operation period when the SWS off-gas is treated, also during
upsets and low capacity operation. At turndown conditions (amine gas 20% and
SWS off-gas 100%), the temperature in the combustion chamber is still sufficient for
complete conversion of ammonia.
3.2.4
Draining K.O. Drums

The amine gas feed and SWS gas feed are passed through their respective K.O.
drums 13D-02 and 13D-01 in order to separate any condensate and entrained
liquids from the gas. Condensate can be present due to tracing failure and liquids
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can be entrained because of inadequate operation in the upstream units. Normally

the feed gas is dry and free from liquids.
3.2.5
Points for Consideration

The aim of this section is to highlight some important aspects.
General
Sudden temperature changes should be avoided whenever possible, since they
might cause leaks at flanges or loosening of iron sulfide scale from the
equipment walls.
H2S and SO2 are extremely poisonous gases. Utmost care must be taken to
avoid exposure of personnel and environment to these gases, e.g. when
draining H2S containing liquid or when taking gas samples.
In special circumstances, protective masks must be worn (see Section 7).
The lower and upper explosion limits of H2S in a gas-air mixture are 4.3 and
45.5 vol.%, respectively. In the stoichiometric ratio with air, it explodes violently
when ignited.
At a temperature of approximately 230C, auto-ignition of liquid sulfur will occur

when in contact with air. Sulfur dust will ignite at approximately 190C.
The boiler water in the waste heat boiler and sulfur condensers should be
sampled periodically to check the concentration of solids.
The maximum allowable total concentration of solids in the waste heat boiler is
3000 ppm, of which a maximum 250 ppm of suspended solids is permitted. The
maximum allowable total concentration of solids in the sulfur condensers is
3500 ppm with maximum 300 ppm of suspended solids.
Higher figures might lead to dirt and scale deposition and finally to damage of
the boiler and condensers. The concentration of solids can be adjusted by
varying the blowdown rate.
All steam traps should be checked frequently to ensure a proper heating

performance. In this way plugging of the process lines, equipment and valves by
solid sulfur can be avoided.
A frequent inspection of the sulfur flow from the sulfur locks and the flame color
as well as reading of the main burner inlet pressure may give an early warning
before plugging by sulfur and/or ammonia salts might occur.
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Main Burner/Combustion Chamber

Care should be taken that the air-to-fuel gas ratio at the main burner is correct.
A major deficiency of air at fuel gas firing might result in deposition of soot on
the first catalyst bed (higher pressure drop and less sulfur conversion). When
the unit is still hot, an air excess might result in equipment damage due to fire
inside the equipment. It might also cause sulfation of the Claus catalyst in the
second reactor, resulting in less sulfur conversion.
Soot can only be removed during a shutdown period by replacing the top layer
of the catalyst bed.
To prevent damage of the burner, it is strongly advised to operate the air side of
the burner at a pressure drop of at least 1.0 mbar.
During the (fuel gas) ignition stage in the burner, the maximum amount of fuel
gas allowed to be present inside the burner/combustion chamber is restricted to
avoid an excessive pressure rise when the actual ignition takes place. For this
reason the burner/combustion chamber are purged before admitting fuel gas to
remove any combustibles that might be left from a previous ignition trial. The
equipment is capable to stay leak tight after a pressure rise during ignition or
explosion, but the internals may be damaged.
No carry-over of liquid hydrocarbons or high amounts of gaseous hydrocarbons

from preceding units should take place as it might damage the main
burner/combustion chamber. It might also cause soot deposition inside the unit,
e.g. on the catalyst beds.
The temperature in the combustion chamber should be at least 1250C in order

to maintain a stable flame. Therefore, the air and acid gas preheaters should
always be in operation.
The windows of the flame scanners and the pyrometer should be cleaned on a
regular basis.
Reactor stages
Runaway temperatures in the Claus reactors should be avoided during hot
standby and shutdown. When the temperature tends to rise to 400C the air-tofuel gas ratio at the main burner should be reduced in order to obtain
substoichiometric conditions. Introduce nitrogen to the reactor for additional
cooling.
Care should be taken that the ratio fuel gas-air and/or acid gas-air at the line
burners is correct. Too little air might result in deposition of soot on the catalyst
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bed (higher pressure drop and less sulfur conversion) and too much air in
sulfatation of the catalyst (less sulfur conversion).
Soot, however, can only be removed during a shutdown period by replacing the
top layer of the catalyst bed.
The performance of the tail gas analyzer should be checked regularly.
Incinerator
The incinerator is started-up before the main burner to convert any hazardous
gas, which might leave the unit during the purging and ignition phases of the
main burner. This does not apply to the initial heating up and drying out phases.
Then the temperature rise of the incinerator should occur gradually and Claus
off-gas from the main burner is required as a cooling medium.
Too high a liquid sulfur temperature should be avoided. Above 155C the
viscosity of the sulfur rises rapidly and may harm the sulfur pumps. Therefore,
the steam coils should only be in operation when no sulfur is produced in the
unit, unless the sulfur temperature drops below 125C.
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3.3
PROCESS CONTROL, ALARM AND SAFEGUARDING SYSTEMS
3.3.1
Process Instrumentation
An extensive number of control instruments, indicators and warning devices are
provided to ensure efficient and safe operation of the unit and to enable a
comprehensive analysis of the unit whilst in operation.
3.3.2
Instrument Alarm System

An alarm system has been installed in order to provide warning of an undesirable
situation arising from abnormal conditions i.e. high or low levels, pressures,
temperatures or flows. When the operator is not able to rectify these conditions,
actions of the automatic safeguarding system prevent dangerous situations.
3.3.3
Safeguarding System
Automatic safeguarding system
A comprehensive logic system has been designed and incorporated in order to
provide maximum protection for personnel, environment and equipment during
startup, shutdown and normal operation steps to avoid creation of dangerous
situations resulting from abnormal process conditions.
The actions of the logic system are described in the Cause and Effect Diagram for
normal operation reference doc. Nr. 20507-64566-13/P.03/0001 and in the
Description of Logic System for Startup and Shutdown Operation, reference doc.nr.
20570-64566-13/P.02/0011.
Emergency shutdown
Emergency shutdown is initiated by actuating either the board mounted or the field
mounted emergency switches in case of extreme situations, not covered by the
automatic safeguarding system, e.g. heavy leakage or plant fire.
3.3.4
Controller, Alarm and Trip Settings

The set points of the process control, alarm and trip instruments are given in the
instrument process data sheets.
3.3.5
Relief Valves
Relief valves are installed to provide adequate equipment protection in case of a
pressure rise.
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3.4
TEMPERATURE RUNAWAYS
3.4.1
Fire inside the Claus Reactors

During the shutdown phase and hot standby operation a rapid temperature rise in
one of the catalyst beds (temperature runaway) may occur when too much air is
supplied to the main burner. Then the sulfur, absorbed in the catalyst, reacts
violently with the oxygen in the air, resulting in a fire. When this happens, the air
supply to the main burner should be decreased and/or the fuel gas supply should be
increased to stop the air break-through from the burner. The corresponding steam
reheater should be stopped. When available, nitrogen should be introduced directly
into the reactor. When the temperature is dropped, the steam reheater can be
restarted.
3.4.2
Fire in the Sulfur Pit

A fire in the sulfur pit is detected by the temperature alarms in the air space of the
sulfur pit. The fire should be extinguished by injection of smothering steam.
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4.0
COMMISSIONING
4.1
INTRODUCTION
A systematic program of startup preparations must be drawn up and carried out to
ensure that the startup properly proceeds with the minimum delay. This is
particularly important when the unit has to be brought on stream together with other
units within a limited period.
The activities during the commissioning period are:
1. The construction of the plant as a whole must be checked in detail against
design and equipment specifications.
2. Chemical cleaning (boiling-out) of the waste heat boiler.
3. Commissioning of utility systems, instrumentation and testing of running
equipment.
4. Natural/Fuel gas intake and drying-out.
5. Loading of catalyst.
6. Heating-up and preparation for startup.
The unit area should be cleaned of all unnecessary construction materials, which
might burn, and the area around the unit should be cleared sufficiently to provide
complete safety of movement for operating and fire fighting personnel. This should
be carried out before the introduction of natural/fuel gas into the plant equipment. All
fire fighting and gas protection facilities within the unit should be available for
immediate use.
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4.1.1
CLEANING OF WASTE HEAT BOILERS AND CONDENSERS
4.1.1.1
Waste Heat Boiler

During the construction period of the unit, the inside of the equipment is exposed to
grease and oil. These have to be removed from the steam side of the waste heat
boiler before the initial startup takes place, as they decrease the heat transfer at the
tubes.
Also scales have been formed on the metal walls. These have to be removed to
avoid dirt accumulation inside the boiler and to avoid harm to the downstream steam
piping and equipment. Following procedure can be executed to clean the boiler or
alternatively a procedure from the boiler manufacturer can be used.
The cleaning of the waste heat boiler takes place in two steps.
In the first step grease and oil are removed and in the second step scale.
First step (removal of grease and oil)
1. Prepare a quantity of Na3PO4, corresponding with 0.3 wt.% and NaOH,
corresponding with 0.025 wt.% in the boiler water.
2. Supply boiler feed water to the boiler until normal level is reached. Keep the
vent open.
3. Add the above-mentioned chemicals to the water content via a manhole etc.
and close the manhole. The vent remains open.
4. Supply the MP steam to the boiler. Keep the water boiling for 24 hours at
atmospheric pressure. Maintain the water level by blowing-down some boiler
water each 1-2 hours.
5. Close the steam supply and drain the total boiler content.
Second step (removal of scale and rust)

1. Prepare a quantity of Na3PO4, corresponding with 0.5 wt.% in the boiler water.
2. Supply boiler feed water to the boiler until normal level is reached. Keep the
vent open.
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3. Add the Na3PO4 to the water content via a manhole etc. and close the manhole.
The vent remains open.
4. Supply LP steam via the steam hose to the boiler. Close the vent when steam is
discharged. Let the pressure rise to LP steam refinery pressure and close the
steam supply. Maintain the water level by blowing-down some boiler water each
1-2 hours. Wait until the pressure has dropped to 1 barg and repeat this step at
least 5 times.
5. After the 5th time of supplying LP steam to the boiler, wait until the pressure has
dropped to 1 barg. Then open the vent. Drain the total boiler content.
6. Clean the boiler by supplying boiler feed water to normal level and drain the
contents. Repeat this several times until the water is clear and has obtained a
pH of approximately 9. If scaling material still comes out of the boiler after
several water washes, it is advised to repeat the scaling removal procedure
(step 2). Make sure that no air can enter the boiler after the cleaning (new rust
formation). Air ingress can be prevented by keeping the boiler under nitrogen
pressure or steam pressure. During cleaning with water, special attention should
be paid to removal of scale and rust at instrument connections.
4.1.1.2
Sulfur Condensers
Removal of scale is not required. Therefore only the removal of oil and grease is
applicable.
Follow the method as described in Step 1 for the Waste Heat Boiler. The steam
supplied should be LP steam instead of MP steam. On conclusion, clean the
condenser by supplying boiler feed water to normal level and drain the contents.
Repeat this several times until the water is clear and has obtained a pH of 9.
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4.1.2
COMMISSIONING OF UTILITY AND INSTRUMENT SYSTEMS

The following recommendations are suggested for the commissioning phase of the
Sulfur Recovery Unit and can be utilized for subsequent startups after routine major
overhauls.
1. It is assumed at this stage that:
Cleaning of lines and vessels has been carried out.
All isolating valves located within the unit are closed and the necessary
blinds at the battery limit installed.
Power and utilities are available.
All running equipment has been checked for lubrication and correct rotation.
Acid gas lines and natural gas lines are cleaned, purged and filled with
nitrogen.
The sulfur degassing vessel has been cleaned and is ready to receive
product.
All hand valves in the steam and condensate lines at the steam preheaters
and the steam reheaters are closed.
The steam and condensate systems are available.
2. Personnel from the Instrumentation Department will check out in detail the
Instrumentation of the Unit to ensure that:
Safeguarding systems function correctly by simulation of abnormal
conditions.
The DCS is properly programmed and contains correct parameters.
All alarms function correctly by simulation of abnormal conditions.
All controllers function correctly by simulation of operating conditions and are
already tuned where possible.
All instruments are commissioned.
3. Testing of the air blowers is advised at this stage so that any mechanical defects
may be rectified. Reference is made to the manufacturer's instruction for
blowers for testing and commissioning.
Simultaneously with the blower testing the unit is blown-through for 60 hours as
the air flow through the plant equipment will remove traces of dust etc., which
has possibly remained in the pipe work from the construction period. In addition,
the air flow will help to pre-dry the fire bricks and refractory linings.
Open the air supply to the main burner with RBV-045. Adjust an initial air flow
rate of 30% on FCV-047 trim air controller. Gradually increase the air flow to
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maximum. Repeat the same, then using the main air controller FCV-046.
What about air lines to Incinerator, Degassing Vessel and jump over line.
When the blow-through/testing operation is completed, the air supply to the
burner is closed with RBV-045. Shutdown the blowers.
4. Check the positions of all non-return valves located in the steam pipe work,
associated with the boiler, condensers and steam heaters. Grease and exercise
all valves, especially plug valves.
Ensure that all level gauge glasses and instruments are clean.
5. It is strongly advised to strip down the burner and ignition lance for cleaning.
Check the burner sight glasses.
6. Slowly supply MP steam to the plant heating system (5LP Header), utilising the
Desuperheater 13DS-2 with LP Condensate (Hot Water) acting as the quench.
However, before systematically commissioning each individual steam trap, open
all low drain points, thereby flushing any dirt out of the pipe work.
When the condensate emitting from the above mentioned drain points run clean,
the steam traps are commissioned and the drain valves are closed, thereby
directing all condensate to the condensate system.
Ensure that the condensate disposal system has been commissioned.
7. Check all steam traced and steam jacketed equipment and lines for heating
efficiency, using thermal crayon or a lump of sulfur.
8. Ensure all valves downstream of the isolating blinds of the boiler feed water
supply lines situated at the battery limit are closed and reposition the isolating
blinds to open position.
9. Commission boiler feed water to the waste heat boilers and the sulfur
condensers as follows:
Waste heat boilers 13E-01/11
Ensure that all boiler feed water valves at the waste heat boiler are closed.
Commission the level control loop of the waste heat boiler. The control valve
will open.
Open fully the battery limit valve of the boiler feed water supply line.
Open the vent on the waste heat boiler.
Open cautiously the block valve upstream the control valve and flush clean
the boiler feed water line up to the bleeders of the control valve until the
water becomes clear.
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Open fully the valves located downstream of the control valve, with the
exception of the block valve. Make sure that the bypass is closed.
Open slightly the block valve in the boiler feed water line at the waste heat
boiler to prevent hammering and start filling.
Open the drain valve of the waste heat boiler to drain initial dirty water, until
the water becomes clear.
Close the drain valve and establish a normal operating level.
Maintain a constant check on the level gauge during filling. The low level
alarm lights will be automatically extinguished. When the control valve is fully
closed, fully open the block valve at the waste heat boiler.
1st, 2nd, 3rd Sulfur condensers 13E-02/04/06
The following applies to combined 1st, 2nd, and 3rd sulfur condensers 13E02/04/06.
Ensure that all boiler feed water valves at the condensers are closed.
Commission the level control loops of the condensers. The control valves will
open.
Open fully the battery limit valve of the boiler feed water supply line.
Open the vents on the condensers.
Open the block valve upstream the control valve and flush clean the boiler
feed water line up to the bleeders of the control valve until the water
becomes clear.
Open fully the valves (located downstream of the control valve, with the
exception of the block valve. Make sure that the bypass is closed.
Open slightly the block valve in the boiler feed water line at the condensers to
prevent hammering and start filling.
Open the drain valve of the condensers to drain initial dirty water, until the
alarm lights will be automatically extinguished. When the control valve is fully
closed, fully open the block valve at the condenser.
4th Sulfur condenser
Ensure that the globe valve in the boiler feed water supply line at the
condenser is closed. Open the block valve near the condenser inlet.
Open the vent on the condenser.
Open slightly the globe valve in the boiler feed water line to prevent
hammering and start filling.
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Open the drain valve of the condenser to drain initial dirty water, until the
alarm lights will be automatically extinguished. When the normal level has
been established, the globe valve in the boiler feed water line should be
closed.
11. Ensure that sulfur lines, sulfur locks and sulfur pit are completely free of foreign
materials.
12. Fill all sulfur locks with solid or liquid sulfur by removing the top blind flange.
Ensure that the individual locks are completely filled before re-installing the blind
flanges.
13. Ensure that the discharge valves of the sulfur pumps and valves in the sulfur
rundown lines are closed.
14. Leak testing of the unit has to be carried out with nitrogen or maximum available
air blower pressure.
Special attention should be paid to the acid gas feed system.
15. Check if the igniter functions properly by testing it outside the burner.
16. Commission the following control loops:
Temperature control loops of the reactor inlets (TCV-078, TCV-089, and
TCV-098).
Steam pressure controllers of the 4th condenser 13E-08: PC-106, acting on
the steam condenser and PC-411B, acting on the steam blow-off line. The
initial set point of PC-411A should be 1.8 barg.
Pressure controllers in HP steam and 5LP steam.
Relevant loops in the utility systems.
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4.2
NATURAL GAS INTAKE AND DRYING OUT
4.2.1
Introduction
Prior to the initial startup phase of the unit, it is necessary to accomplish a complete
drying out of the reaction furnace and incinerator. This is performed by increasing
the temperatures at a controlled rate of 15 to 20C per hour, until a temperature of
300C is reached.
After about 52 hours the drying out phase is complete (see figure 2) and the heating
up of the reaction furnace can be continued until the operating temperatures are
reached.
Next, the unit is cooled-down to enable loading of the catalyst.
In the initial startup phase, the incinerator should only be started when the Claus
section produces an off-gas, as this gas acts as a cooling medium allowing for a
gradual heating-up of the thermal incinerator. Once the incinerator is hot, it can be
operated without Claus tail gas.
Remarks
1. The drying-out and heating-up procedures as described below, indicated in
figure 2, are to be considered as guidance only. The refractory lining
manufacture should supply dedicated drying out curves for all refractory.
Simplified Outline
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
Remove all isolating blinds, except for feed gases and oxygen.
Reset the logic system.
Start the air blower.
Commission the remaining utility systems.
Dry-out the unit with hot air.
Purge the main burner with nitrogen.
Admit natural gas to the main burner.
Start the reheaters of the catalytic reactors.
Start the incinerator burner.
Further dry-out and heat-up the unit.
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4.2.2
Detailed Outline
Preparations
1. All isolating blinds situated at the unit and battery limits are removed, except at
acid feed gas lines.
2. Check the permissives to start the main burner.
Check the liquid level in the waste heat boiler (LT-072/073).
Ensure that natural gas for the main burner is available (PI-061).
Ensure that the emergency shutdown switches HY-070/071 and RBV064/066 are in the correct position.
3. Reset the logic system for the main burner by HS-217.
4. Start one of the air blowers. Confirm that the blower vents properly to the
atmosphere to prevent surging.
5. Commission all utility systems.
6. Open the air supply to the main burner with RBV-045. Adjust an initial air flow
rate of 30% on FCV-047 trim air controller. Gradually increase the air flow to
maximum. Repeat using the main air controller FCV-046.
4.2.2.1
Purging and ignition in the main burner

The ignition sequence is started with the nitrogen purge of the main burner and
proceeds automatically until ignition is obtained. Within 15 minutes after purging, a
flame should be established.
1. Commission the nitrogen for purging to prevent sooting of the flame scanners
and sight glasses.
2. Start the ignition procedure by actuating button HS-218.
Purging of the main burner is started automatically. Ensure that the nitrogen flow
is above the trip setting of BALL-050. The purge is completed after 5 minutes.
3. When the purge is completed, the next step is automatically started. The igniter
is inserted, the combustion air supply is started, the igniter is energized and the
natural gas valves are opened. Within 5 seconds ignition should be obtained,
otherwise the unit is tripped.
The air flow rate is normally the minimum allowable air flow to the burner. In
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case ignition is hard to obtain with this flow rate, it can be manually increased
within a certain range by varying the output of controller FCV-046/047. The
natural gas flow rate is such that the combustion is stoichiometric. In addition,
the natural gas flow (FCV-062) can be manually adjusted within a certain range.
The settings are determined empirically.
Remark
Normally the burner can be started quickly with the predefined positions on the
air and natural gas controllers. These settings correspond with stoichiometric
combustion at the minimum air flow with the corresponding natural gas flow.
However, due to the actual burner dimensions and location of the tip of the
igniter, it is sometimes easier to obtain ignition at other flow rates. This should
be empirically found. Once these flow rates have been adjusted in the DCS,
they can be used for subsequent startups.
4. One minute after ignition following controllers are accessible for the operator.
FCV-047, acting on the trim air valve.
FCV-046, acting on the main air valve.
FCV-062, natural gas.
5. After establishing a stable flame, the size of the flame should be restricted.
Decrease the natural gas flow to its minimum value of 18 kg/h and adjust the air
flow to 987 kg/h. This results in a 330% of stoichiometric burn, i.e. with 230%
excess air.
Switch FCV-062 (natural gas) and FC-046 (combustion air) to AUTO mode.
After switching FC-046 to CASCADE, the ratio between natural gas and air can
be adjusted with HS-206. FC-047 can be taken into operation to allow the
operator to increase the air flow during warming-up.
4.2.2.2
Heating of the first Claus Reactor

1. Commission HP steam to the first steam reheater 13E-03 and commission its
condensate system. Ensure that control valve and downstream block valve in
the steam supply line is fully closed.
Put the heater carefully into operation by opening control valve TCV-078 and
slowly opening the downstream block valve. Do not open the control valve until
the heater is sufficiently heated!
2. Commission the automatic temperature control system (TC-251). Keep the
temperature at TC-251 between 150C and 180C during the first six hours in
order to obtain a gradual heating-up of the reactor.
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4.2.2.3
Heating of the second Claus Reactor

1. Commission HP steam to the second steam reheater 13E-05 and commission
its condensate system. Ensure that control valve and downstream block valve in
the steam supply line are fully closed.
temperature at TC-089 between 150C and 180C during the first six hours In
4.2.2.4
Heating of the third Claus Reactor

1. Commission HP steam to the third steam reheater 13E-07 and commission its
condensate system. Ensure that control valve in the steam supply line is fully
closed.
temperature at TC-098 between 150C and 180C during the first six hours In
4.2.2.5
Start of incinerator
When the main burner is in operation, sufficient off-gas is produced to start heatingup procedure of the incinerator.
Reference is also made to the Safeguarding narrative.
Document no 20507-64566-13/P.02/0015
1. Check the permissives to start the incinerator burner.
Check the liquid level in the incinerator waste heat boiler (LT-179/180).
Ensure that fuel gas for the incinerator burner is available (PT-159).
Ensure that the emergency shutdown switches are in the correct position
(HS-166/167 for the incinerator).
2. Reset the logic system for the incinerator by HS-257.
3. Start the incinerator air blower. Confirm that the blower vents properly to the
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4. Commission the instrument air supply for purging to prevent sooting of the flame
scanner and sight glasses.
5. The ignition sequence is started with an air purge of the incinerator and
proceeds automatically until ignition is obtained. Open RBV-144 by actuating
HS-258. Ensure that the air flow is above the trip setting of FALL-147. The
purge is completed after 3 minutes.
is inserted and energized and the fuel gas valves are opened. Within 5 seconds
ignition should be obtained, otherwise the unit is tripped.
In case ignition is hard to obtain at the pre-defined air flow rate, it can be
manually increased within a certain range by varying the output of controller
FCV-146. The fuel gas flow rate is such that the combustion is stoichiometric. In
addition, the fuel gas flow (FCV-160) can be manually adjusted within a certain
range. The settings are determined empirically.
Remark
air and fuel gas controllers. These settings correspond with stoichiometric
combustion. However, due to the actual burner dimensions and location of the
tip of the igniter, it is sometimes easier to obtain ignition at other flow rates. This
should be empirically found. Once these flow rates have been adjusted in the
DCS, they can be used for subsequent startups.
FCV-146, primary air.
FCV-148, staged air.
FCV-160, fuel gas.
Decrease the fuel gas flow to its minimum value of 29 kg/h and adjust the air
flow to 356.5 kg/h. This results in a 330% of stoichiometric burn, i.e. with 230%
excess air. Switch FCV-160 (fuel gas), FCV-146 (primary air) and FCV-148
(staged air) to AUTO mode.
After switching FCV-146 to CASCADE, the ratio between fuel gas and air can
be adjusted with HC-160C. The staged air flow on FCV-148 should initially be
maximum to provide as much cooling as possible.
Remark
During the initial startup the off-gas from the main burner provides sufficient cooling,
so that a gradual heating-up is obtained. Once the refractory in the incinerator is
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dried-out, a faster temperature rise is allowed. Therefore, at the next startup the
incinerator is started before the main burner.
4.2.2.6
Drying out and heating up of the combustion chamber

1. After about 52 hours the drying out phase is complete (see figure 2) and the
heating up of the combustion chamber can commence.
The combustion chamber is heated up to about 1000C at a rate of 20C per
hour by adjusting the air and natural gas flows to the main burner.
To restrict the temperature rise, quenching steam should be admitted to the
burner. The steam supply is started with HS-220, but not before all temperatures
in the unit exceed 100C.
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2. The generation of steam from the waste heat boiler starts with increasing heat
input. When a large amount of steam is exhausted, the vent is closed.
Check again that the condensate disposal system has been correctly
commissioned.
4.2.2.7
Drying-out and heating-up of the reactor stages

1. During the first 24 hours of operation, the outlet temperature of the reheaters
should be limited to 150-180C.
After this period the reactors are heated to the maximum temperature that can
be obtained with the reheaters at 15C - 20C per hour.
2. The generation of steam from the condensers starts gradually. Both the
condensors13E-02/04/06 shared in one shell and 13E-08. When a large amount
of steam is exhausted, the vent is closed. Operate the condensers at their
normal operating pressure.
4.2.2.8
Drying out and heating up of the incinerator

After about 52 hours the drying out phase is complete (see figure 2) and the heating
up of the incinerator can commence.
The incinerator is heated up to about 700C at a rate of 10C per hour by adjusting
the air and natural gas flows to the burner, as well as the staged air flow.
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Figure 2: drying out & heating up (to be confirmed with refractory vendor information)
Temperature
1200C
drying-out
heating-up
1000C
800C
Comb. Chamber
Incinerator
600C
400C
Claus reactors
SUPERCLAUS reactor
200C
0C
0
20
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40
52
60
80
100
Time (hours)
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120

4.3
CATALYST LOADING
After the initial drying-out and heating-up procedure, the unit is shut down to allow
opening of the equipment to start loading of catalyst into the reactors.
4.3.1
Stopping the unit

1. Decrease gradually the temperature in the combustion chamber by reducing the
natural gas supply. Adjust an excess of air of approximately 200%.
2. Cool down the catalyst beds of the reactors by shutting-off the steam reheaters.
3. Close the steam supply to the 4th condenser and the blow-down valve.
4. The unit will gradually cool down.
5. Close the natural gas supply to the main burner with HS-219. The air is
automatically tripped as well.
6. Shutdown the incinerator.
8. Open the air supply to the main burner with HS-206. Adjust an initial air flow
rate of 30% on FC-046. Gradually increase the air flow to maximum. Both
control valves FCV-046 and FCV-047 can be used.
9. Install spectacle blinds in the natural gas at the battery limit.
10. When the temperature is no longer decreasing, open the upper manhole on the
reactor.
11. As soon as the reactor temperatures are sufficiently low, catalyst loading can
take place.
A Subsidiary of Jacobs Engineering Group Inc.

Trade register: Rijnland 24301248

4.3.2
Catalyst loading
1. Remove the pipe or bellow between the reactor outlet and the condenser inlet
and place a temporary blind at the condenser inlet. In this way, no catalyst dust
will come into the condenser.
2. Check the interior of the reactor for cleanliness, with particular attention to the
area beneath the support grid.
3. Indicate on the wall the required heights for ceramic balls and catalyst. The
height of the catalyst bed is approximately 10% higher than indicated on the
data sheet. After some time of operation, the bed height specified in the data
sheet will be obtained as the catalyst density will increase to the normal bulk
packed density.
4. First reactor
From the top of the grid support, the following heights are applicable:
Bottom layer (support balls): indication at 100 mm.
The bottom layer (height: 100 mm) consists of 6 mm ceramic balls for
support of the catalyst bed.
Bottom catalyst layer (CRS-31): indication at 814 mm.
The bottom catalyst layer (normal height: 740 mm) consists of CRS-31
catalyst. Initially the catalyst bed is 10% higher than indicated on the
equipment drawing. The catalyst will shrink to its normal height after some
time of operation.
Top catalyst layer (CR-3S): indication at 286 mm.
The top catalyst layer (normal height: 260 mm) consists of CR-3S catalyst.
Initially the catalyst bed is 10% higher than indicated on the equipment
drawing. The catalyst will shrink to its normal height after some time of
operation
5. Second reactor
Catalyst layer (CR-3S): indication at 1100 mm.
The catalyst layer (normal height: 1000 mm) consists of CR-3S catalyst.
operation.
6. Third reactor
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Catalyst layer (CR-3S): indication at 1100 mm.
The catalyst layer (normal height: 1000 mm) consists of CR-3S catalyst.
operation.
7. On completion of catalyst loading, check that the surface area has been
leveled. Measure in several places inside each reactor the height of the free
space from the catalyst surface to the top of the reactor.
8. After the first reactor has been loaded, dust and fines should be removed by an
air flow from the blower through the reactor. Next, the reactor is closed.
9. Reinstall the pipe or bellow between the reactor and condenser.
10. Removal of dust from the second reactor should take place when the first
reactor has been closed. This is repeated for all reactors.
11. Make a report of the catalyst loading, mention the number of drums and take
samples of the catalyst. Do the same for the ceramic balls.
12. After catalyst loading and leak testing of the reactors, the unit is heated up
again.
General remarks
Care must be taken to minimize the creation of catalyst fines during the loading
of the reactors. Catalyst dust and fines are to be removed with the help of an air
flow through the reactor.
For this reason, the pipe between reactor outlet and condenser inlet should be
removed and a temporary blind at condenser inlet should be installed.
This procedure has to be followed for each reactor separately.
During catalyst loading some dust is produced which should not be inhaled.
Personnel who are outside the reactor during loading should wear dust masks.
Inside the reactor, a positive pressure air mask should be worn. Eye contact
and prolonged skin contact with the catalyst should be avoided by wearing the
relevant protective clothing.
The catalyst bed heights indicated on the reactor walls are approximately 10%
higher than indicated on the equipment drawings. After some time of operation, the values of
the equipment drawings will be obtained when the catalysts have been settled.
The catalyst should be protected against water.
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5.0
STARTUP
5.1
HEATING UP AFTER SHUTDOWN

Preparations
1. Ensure that the unit is leak-tight, that all utility systems are commissioned and
that equipment is ready for startup (e.g. sufficient levels in waste heat boilers
and condensers).
2. Ensure that the sulfur locks are filled with sulfur.
3. All isolating blinds situated at the unit and battery limits are removed, except at
the acid feed gas lines.
Start of incinerator
1. Check the permissives to start the incinerator burner.
Check the liquid level in the incinerator waste heat boiler (LYLL-180).
Ensure that fuel gas for the incinerator burner is available (PYLL-272).
Ensure that the emergency shutdown switches are in the correct position (HS166/167).
2. Reset the logic system for the incinerator by HS-257.
3. Start the incinerator air blower. Confirm that the blower vents properly to the
4. Commission the instrument air supply for purging to prevent sooting of the
flame scanner and sight glasses.
5. The ignition sequence is started with an air purge of the incinerator and
proceeds automatically until ignition is obtained. Open RBV-144 by actuating
HS-258. Ensure that the air flow is above the trip setting of FYLL-147. The
purge is completed after 3 minutes.
is inserted and energized and the fuel gas valves are opened. Within 5 seconds
ignition should be obtained, otherwise the unit is tripped.
In case ignition is hard to obtain at the pre-defined air flow rate, it can be
manually increased within a certain range by varying the output of controller
FC-146. The fuel gas flow rate is such that the combustion is stoichiometric. In
addition, the fuel gas flow (FC-256) can be manually adjusted within a certain
range. The settings are determined empirically.
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FC-146, primary air.

FC-148, staged air.
FC-256, fuel gas.
Decrease the fuel gas flow to its minimum value of 18 kg/h and adjust the air
flow to 987 kg/h. This results in a 330% of stoichiometric burn, i.e. with 230%
excess air.
Switch FC-256 (fuel gas), FC-146 (primary air) and FC-148 (staged air) to
AUTO mode.
After switching FC-256 to CASCADE, the ratio between fuel gas and air can be
adjusted with HC-160B. The staged air flow on FC-148 should initially be
maximum to provide as much cooling as possible.
9. When the temperature in the incinerator is sufficiently high (250C) FC-256 is
switched to CASCADE.
Start of main burner

1. Start one of the air blowers. Confirm that the blower vents properly to the
2. Check the permissives to start the main burner.
Check the liquid level in the waste heat boiler (LYLL-073).
Ensure that natural gas for the main burner is available (PYLL-060).
4. Commission the nitrogen for purging the flame scanners and sight glasses to
prevent sooting.
5. The ignition sequence is started with the nitrogen purge of the main burner and
proceeds automatically until ignition is obtained. Within 15 minutes after
purging, a flame should be established.
Start the ignition procedure by actuating button HS-218. Ensure that the
nitrogen flow is above the trip setting of FYLL-058. The purge is completed after
5 minutes.
is inserted, the combustion air supply is started, the igniter is energized and the
natural gas valves are opened. Within 5 seconds ignition should be obtained,
otherwise the unit is tripped.
The air flow rate is normally the minimum allowable air flow to the burner. In
case ignition is hard to obtain with this flow rate, it can be manually increased
within a certain range by varying the output of controller FC-046/047. The
natural gas flow rate is such that the combustion is stoichiometric. In addition,
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the natural gas flow (FC-062) can be manually adjusted within a certain range.
The settings are determined empirically.
Remark
air and natural gas controllers. These settings correspond with stoichiometric
combustion at the minimum air flow with the corresponding natural gas flow.
However, due to the actual burner dimensions and location of the tip of the
igniter, it is sometimes easier to obtain ignition at other flow rates. This should
be empirically found. Once these flow rates have been adjusted in the DCS,
they can be used for subsequent startups.
FC-046, acting on the trim air valve.
FC-047, acting on the main air valve.
FC-062, natural gas.
8. After establishing a stable flame, the size of the flame is restricted. Decrease
the natural gas flow to its minimum value of 18 kg/h and adjust the air flow to
987 kg/h. This results in a 330% of stoichiometric burn, i.e. with 230% excess
air.
Switch FC-062 (natural gas) and FC-046/047 (total air) to AUTO mode.
After switching FC-062 to CASCADE, the ratio between natural gas and air can
be adjusted with HC-062. FC-047 can be taken into operation to allow the
operator to increase the air flow during warming-up.
Heating of the Claus Reactors

1. Commission HP steam to the steam reheaters 13E-03, 13E-05 and 13E-07.
Commission their condensate systems. Ensure that the control valves in the
steam supply lines are fully closed.
Put the heaters carefully into operation by slowly admitting steam via the control
valve bypass. Do not open the control valve until the heater is sufficiently
heated!
2. Commission the automatic temperature control systems (TC-078, TC-089 and
TC-098). The reactors are heated at a rate of 15-20C per hour until a top
temperature of 240C is reached.
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Remarks
Please note that the above procedure only applies when the unit does not
contain sulfur, since excess air is introduced. At temperatures above 200C in
combination with the presence of sulfur, excess air may lead to sulfur fires.
Reference is made to Section 2.5 "Actions in case of automatic shutdown
(Trip)" for the startup procedures in case sulfur is present in the unit.
The presence of sulfur in the unit after a shutdown should be avoided.
Reference is made to Section 2 for the proper shutdown procedures.
After a trip, the unit is brought on-stream as soon as possible. Then the unit is
still hot, so introduction of excess air for cooling is not required and should be
avoided. Natural gas shall be burnt substoichiometrically, see also remark a).
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5.2
CHECK LIST AND PREPARATION BEFORE FEED GAS INTAKE

Confirm that following items have been completed before feed gas intake.
1. Open the sulfur outlets of the sulfur condensers and coalescer.
2. Commission HP steam to the air and acid gas preheaters and commission their
condensate systems. Put the heaters carefully into operation: admit slowly
steam to the heaters.
3. Confirm steam supply to the steam tracing and jacketing by means of
temperature indicating stick for 125C or lumps of sulfur.
4. Check all steam traps, especially at the jackets of sulfur run-down lines.
5. Remove the blinds in the acid feed gas feed lines. The battery limit valves
remain closed.
6. Check the burner flanges and sight glasses for leaks.
7. Check the availability of the following Drger tubes for tail gas analyses:
Component(s)
Range
H2S
0.2 - 7
vol.%
H2S
(H2S + SO2)
SO2
O2
100 - 2000
0.2 - 7
50 - 8000
5 - 23
ppm vol
vol.%
ppm vol
vol.%
8. Prepare safety measures before startup:

Make at least 4 air masks available.
Make air bottle available for refilling of air mask bottles or make air supply
lines with filter available, depending on the type of the mask.
Check wind direction.
Provide operating personnel with portable H2S detectors (personnel
protection).
Close to sulfur plant area to personnel during startup, except for operating
personnel.
9. Ensure that the burners are in stable operation and on automatic control.
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10. Check following temperatures and pressures:

Combustion chamber
Claus reactors inlet
Incinerator
1000 - 1300
240
750 - 800
C
C
C
11. Check the supply of air and nitrogen for purging the flame scanners and the
sight glasses.
12. Make tools such as locks, keys, valve handles, wrenches, sealing tape and
soap for leak testing available.
13. Check if the H2S monitor for personnel protection has been commissioned and
set at the correct alarm setting.
14. Ensure that the sulfur locks are filled with liquid sulfur.
15. Commission the tail gas H2S/SO2 analyzer.
16. Take care that a portable O2 analyzer for stack gas is available.
17. Check the level in the Acid gas knock-out drum 13D-01.
18. Check the level in the Sour gas knock-out drum 13D-02.
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5.3
FEED GAS INTAKE
5.3.1
Simplified Outline
Adjust the air and natural gas flows to the main burner
Adjust the "air-to-amine acid feed gas" ratio as well as the "air-to-SWS acid
feed gas" ratio.
Admit amine acid feed gas to the main burner.
Switch the flow control for the amine acid feed gas to AUTO and gradually
increase its feed gas flow.
Stop the natural gas supply to the main burner when desired.
Regenerate the Claus catalyst if required.
Increase the feed gas flow to the maximum available quantity.
Adjust the inlet temperatures of the Claus reactors to design conditions.
Admit SWS acid feed gas when desired.
1.
2.
3.
4.
5.
6.
7.
8.
9.
5.3.2
Detailed Outline
Adjusting air and natural gas
Adjust the natural gas combustion in the main burner to 95% of stoichiometric
combustion (HC-062). Note that FC-062 is in CASCADE mode and that FC-047
should be switched to CASCADE before feed gas intake.
Taking in Amine acid feed gas

1. Pre-adjust the air to acid gas ratio for HC-018 (Amine acid feed gas) to 1.9 kg
air/kg feed gas, for case 1. For case 3, the total acid gas feed is formed by the
amine acid gas feed and the SWS acid gas feed. The amine acid gas feed has
an air to acid gas ratio for HC-018 of 1.4 kg air/ kg feed gas and the SWS acid
gas feed has an air to feed ratio for HC-023 of 1.9 kg air/kg feed gas.
2. Open the battery limit valves in the Amine acid feed gas and SWS acid feed gas
feed lines.
3. Start the Amine acid feed gas supply to the main burner with HS-202.
4. Within 30 seconds the feed gas flow must be established. The air flow follows
automatically the feed gas flow. The initial feed gas flow for case 1 is 700 kg/h
and for case 3 this is 815 kg/h (20% of the design flow).
5. 60 seconds after establishing the Amine acid feed gas flow, the flow controller
FC-018 becomes accessible for the operator. Switch it to AUTO mode.
6. Increase the feed gas flow to 30% by adjustment of the set point of FC-018.
The air flow will follow automatically.
7. Increase the feed gas flow to 40%.
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8. Switch AC-111 to AUTO mode and maintain the (H2S-2SO2) value at -0.5 vol.%
9. Check the H2S content in the process gas from the fourth condenser with
Drger tubes and compare this with the H2S analyzer.
10. Ensure that sulfur is running by opening the funnels. Use air masks and eye
protection equipment, refer to Section 7.2.
11. Check the O2 content of the incinerator flue gas with Drger tubes or portable
analyzer. It should be approx. 1.6 vol.%.
12. As soon as the unit runs stable, the natural gas supply to the main burner can
be stopped.
Decrease the natural gas flow with FC-062.
Stop the natural gas supply with HS-219 and close the quenching steam in
case it was in operation.
Note that the temperature in the combustion chamber must be kept above
930C when firing H2S acid gas in order to have a stable flame.
13. Increase the amine feed gas flow to maximum. When desired switch FC-018 to
CASCADE with the pressure controller that is located in the amine unit.
14. Decrease the Claus reactor inlet temperatures to the normal value of 240C
(first reactor), 210C (second reactor) and 195C (third reactor).
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5.4
STARTUP OF SULFUR DEGASSING SYSTEM

It is assumed that the degassing system is commissioned.
5.4.1
Initial Startup or Startup after a Long Shutdown

Both FCV-113/116 should initially be in operation to obtain a high vent air flow rate,
since a high amount of H2S is released immediately after admitting the stripping air.
1. Reset the degassing logic system with HS-237.
2. Open the steam supply to the sulfur degassing vessel 13D-08. The vent air flow
should exceed the set point of FYL-504A within 60 seconds, otherwise the
steam is stopped.
3. As soon as the bubble columns are completely submerged, the stripping air
supply is started with HS-236. The stripping air flow should exceed the set point
of FALL-117 within 60 seconds. If not, the stripping air is stopped.
Start the pumps 13P01A/B within the bubbles.
4. 60 minutes after starting the stripping air, the logic system allows to close one of
the FCVs. However, it is advised to continue with both FCVs for a few hours
during initial startup, as the degassing process is not efficient as long as the
sulfur level is below its normal value.
5. Check the sulfur temperature in the stripping compartment frequently. It should
be between 130C and 174C near the 2nd bubble.
5.4.2
Startup after Short Interruption

There is no need to start the second ejector after an interruption of the degassing
process of less than one hour. Then the system is restarted according to the
following procedure:
1. Reset the degassing logic system with HS-237.
2. Open the steam supply to the ejectors with HS-503. The vent air flow should
exceed the set point of FALLL-504B within 60 seconds, otherwise the steam is
stopped.
3. Start the stripping air supply with HS-236.
Within 60 seconds the stripping air flow should exceed the set point of FALL117. If not, the stripping air is stopped.
Adjust locally a stripping air flow of 99 kg/h to each.
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5.5
TAKING IN SWS ACID FEED GAS

1. Start the SWS acid feed gas supply with HS-203.
2. Within 30 seconds the SWS acid feed gas flow must be established. The air
flow follows automatically the increased amount of feed gas flow. The initial NH3
acid gas flow is 235 kg/h (20% of the design flow).
3. 60 seconds after establishing the SWS acid feed gas flow, the flow controller
FC-023 becomes accessible for the operator. Switch it to AUTO mode.
4. Increase the SWS acid feed gas flow. When desired switch FC-023 to
CASCADE with the pressure controller that is located in the SWS unit.
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6.0
6.1
SHUTDOWN
GENERAL
A proper shutdown procedure is most important. Sulfation of the catalyst, plugging
after restart and corrosion are mostly the result of misoperation or wrong
procedures during shutdown. Therefore, a scheduled shutdown should be carefully
carried out.
During normal operation sulfur vapor is absorbed in the pores of the Claus catalyst.
Prior to a scheduled shutdown it is necessary to remove the sulfur from the catalyst
to prevent that the sulfur inside the catalyst is exposed to air at elevated
temperatures, which results in runaway temperatures. The procedure also prevents
sulfur solidification inside the catalyst.
For this purpose, the inlet temperatures of the Claus reactors are raised 15C to
30C above the normal operating temperature and operated at this temperature for
48 hours prior to shutdown.
In this way the absorbed sulfur is removed from the catalyst pores and is
subsequently condensed in the sulfur condensers and drained to the sulfur pit. This
operation is called heat soak.
After 48 hours of operation at elevated temperature, the feed gas supply is stopped
and the unit is purged with inert gas.
The inert gas is obtained by substoichiometric combustion (substoichiometric
means shortage of air) of natural gas and air in the main burner. The
substoichiometry can visually be checked by means of the flame color. Blue means
excess air, pink blue means stoichiometric combustion, pink means slightly
substoichiometric combustion and yellow means deep substoichiometric
combustion.
Steam is supplied to the burner to prevent overheating of the reaction furnace.
Moreover, it increases the inert gas flow through the unit. The steam to natural gas
ratio is approximately 4 on weight basis.
During this operation the air flow to the main burner is 68.4 kg/h at a natural gas
flow of 36 kg/h. Steam for cooling is approximately 140 kg/h.
When it is planned to shutdown the unit completely, the inlet temperatures of the
Claus reactors are raised as high as possible during the substoichiometric natural
gas combustion in the main burner. This operation is called sulfur stripping. No
excess air should be introduced via the main burner during this operation as the air
will react with the sulfur on the catalyst which may result in too high a catalyst
temperature and sulfation of the catalyst.
On the other hand, the incinerator should be operated with excess air to convert
any sulfur vapor into sulfur dioxide.
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There are three shutdown procedures to be considered:

1. Shutdown for a short period (hot standby)
The feed gas supply is stopped, but the unit is kept on standby, so that the unit
can be restarted immediately on feed gas. The whole unit is kept hot during this
period; the burners remain in operation on natural gas.
The natural gas at the main burner is burnt substoichiometrically. In this way, an
inert flue gas is obtained for purging the unit. Steam is supplied to the burner for
cooling of the flame.
This shutdown procedure is preferred because formation of corrosion products
is prevented and there is less chance on plugging and on sulfate formation in
the Claus catalyst, which causes deactivation. In this way the unit can be
operated for a few days or even for a few weeks.
It is essential that during hot standby operation, no excess air is
introduced into the plant, as it will result in sulfate formation in the
catalyst and consequently in deactivation of the catalyst.
2. Shutdown for a long period (complete shutdown)
This procedure should be followed in the event the unit has to be shutdown
completely and opened for maintenance or catalyst exchange.
The difference between this procedure and the procedure discussed above is
that now all absorbed sulfur is removed from the catalyst bed and pyrophoric
FeS on the equipment walls is oxidized before the actual shutdown.
This shutdown procedure normally takes four days. It is pointed out that before
excess air is introduced, the unit should be purged by inert flue gas for at least
24 hours and the catalyst beds should be cooled during this period to 200C.
The inert gas flow is produced by substoichiometric combustion of natural gas
in the main burner. During this operation the air flow to the main burner is 987
kg/h at a natural gas flow of 58 kg/h; steam for cooling is approximately 15 kg/h.
It is advised to make a temperature plot of top and bottom temperatures of the
Claus catalyst beds, the outlet temperatures of the reactors, as well as a plot of
the SO2 content in the tail gas from the third reactor.
After 24 hours, excess air is gradually introduced to remove the last traces of
sulfur and to oxidize the pyrophoric FeS, created during normal operation in the
equipment.
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3. Automatic shutdown (trip)

The unit is shutdown either automatically by the safeguarding system or
manually when the shutdown switches in the control room or in the plant are
actuated.
As the unit is hot, there will be enough time to take measures before sulfur will
solidify.
After a trip, the unit shall be brought on stream as soon as possible to avoid the
heating-up procedure of the combustion chamber. This would require excess air
combustion in the main burner, which might harm the catalyst and equipment
when FeS and sulfur are present.
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6.2
6.2.1
SHUTDOWN PROCEDURE FOR SHORT PERIOD (HOT STANDBY)

Simplified Outline
1. Stop the SWS acid gas feed supply and reduce the Amine acid gas feed flow to
30%.
2. Increase the Claus reactor inlet temperatures at 48 hours prior to feed gas shutoff.
3. Commission natural gas and steam to the main burner and shut-off the feed
gas.
4. Keep an eye on the reactor temperatures.
6.2.2
Detailed Outline
Reducing feed gas flows and increasing reactor inlet temperatures
1. Switch FC-023 to AUTO mode and reduce the SWS acid feed gas flow,
followed by a complete stop with HS-203.
2. Switch FC-018 to AUTO mode and reduce the Amine acid feed gas flow to
30%.
3. Increase the inlet temperatures of the first, second and third reactor as high as
possible. Maintain this situation for 48 hours.
4. Open the natural gas supply to the main burner with HS-219. Adjust a flow rate
of 58 kg/h, corresponding with the hot standby flow.
Shut off the feed gas
1. Start the steam supply to the main burner (HS-220) in order to avoid too high a
temperature in the combustion chamber.
2. Stop the feed gas flow with HS-202. By doing so, also AC-111 is switched to
MANUAL mode. The steam supply to the main burner should now be 15 kg/h.
Note that it is essential that the steam to natural gas ratio is approximately 4
(on weight basis).
Maintain the acid gas preheater in operation.
3. Ensure that the combustion in the main burner is substoichiometric.
4. Open the steam supply to the steam coils in the sulfur pit.
5. Close the hand valves in the boiler water supply and return lines of the sulfur
cooler.
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6.3
SHUTDOWN PROCEDURE FOR LONG PERIOD (COMPLETE SHUTDOWN)
6.3.1
Simplified Outline
1. Stop the SWS acid gas feed supply and reduce the Amine acid gas feed flow to
30%.
2. Make the Claus reactor inlet temperatures as high as possible at 48 hours prior
to feed gas shut-off.
3. Commission natural gas and steam to the main burner and shut-off the feed
gas.
4. Raise the Claus reactors inlet temperatures as high as possible and maintain
these conditions for at least 24 hours.
5. Make a plot of the Claus reactor temperatures and the SO2 content in the tail
gas.
6. Reduce the Claus reactor bed temperatures to 200C.
7. Slowly introduce excess air to remove the remaining sulfur and FeS from the
unit.
8. Keep all plant heating systems in operation.
9. Gradually cool down the unit.
6.3.2
Detailed Outline
Initially follow the shutdown procedure for short period (Section 3.2.2).
Strip sulfur from the catalyst
1. Check the natural gas and air supplies to the main burner. The air to natural
gas ratio should be slightly substoichiometric.
Check the O2 content in the flue gas from the main burner.
2. Make the inlet temperatures of the Claus reactors as high as and maintain
these temperatures for at least 24 hours.
3. Keep all plant heating systems in operation.
4. Make a plot of the top, bottom and outlet temperatures of the Claus reactors.
Take readings every 5 minutes for the first hour and every 15 minutes
thereafter.
Make also a plot of SO2 content in the tail gas. Take readings every 10 minutes
during the first hour and every 30 minutes thereafter.
5. If the temperature in a reactor tends to rise above 350C, the corresponding
steam reheater should be shutdown. Restart the steam reheater when the
reactor temperature has dropped below 150C.
If the temperature still tends to rise to 380C, it might be considered to inject
nitrogen into the reactor inlet.
A temperature of 400C is the absolute maximum for the catalyst bed.
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6. Maintain the following temperatures:

Combustion chamber
Claus reactors
Incinerator
1000 - 1400
250
750
C
C
C
Cool down the unit

1. Shut-off the steam reheaters to cool down the Claus reactors.
2. Slowly introduce a small amount of excess air to the main burner as soon as
the catalyst bed temperatures are 200C.
The initial O2 content in the flue gas from the main burner should be
approximately 1%, to be checked by oxygen analyses.
The bed temperatures should be watched for any sign of temperature increase.
Reduce immediately the excess air in the event the temperature shows
indications of rising above 230C.
If the temperature tends to increase towards 350C, it might be considered to
inject nitrogen into the corresponding reactor inlet. The temperature should
never exceed 400C.
3. Start a plot of the Claus reactor temperatures. Read the temperatures every 5
minutes during the first hour of the excess air operation, hereafter every 15
minutes.
Also, make a plot of the SO2 content in the tail gas, reading every 10 minutes
during the first hour of the excess air operation, hereafter every 30 minutes.
4. Gradually cool down the unit by introducing more excess air. Continue to watch
the reactor bed temperatures.
5. Close the sulfur outlets of the sulfur condensers and coalescer.
6. Close the natural gas and steam supplies to the main burner by actuating HS219 (natural gas) and HS-220 (steam). Purge the unit with air so that no wet
process gas has been left in the equipment, which might cause corrosion. Stop
the air supply to the Claus section after purging.
7. Shut-off the main air blower after finishing the sulfur stripping process in the
degassing vessel (refer to Section 3.4).
9. Open the valve in the separation wall between the stripping and the storage
compartments of the sulfur pit.
Empty the sulfur pit and close the valves in the sulfur transfer line to the battery
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limit. When it is necessary to open the sulfur lines and locks, the locks can be
emptied by blowing with steam or nitrogen.
Otherwise, sulfur may be kept as liquid in the sulfur locks by maintaining the
supply of heating steam.
10. Block-off the boiler feed water supply and close the blow down valves at the
waste heat boiler and sulfur condensers.
11. Vent and drain the waste heat boiler and sulfur condensers if necessary.
12. Check if all shutdown valves are closed.
13. Install spectacle blinds at the battery limits, except for the LP steam for internal
heating.
Remark
During the shutdown phase it must be constantly born in mind that a rapid
temperature drop is undesirable because:
Lining materials may be damaged.
High thermal stresses or contraction may deform piping and equipment,
causing leaks after a restart.
Solidification of sulfur may occur.
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6.4
6.4.1
RESTART AFTER AN AUTOMATIC SHUTDOWN (TRIP)

As soon as the cause of the trip has been rectified, the unit should be restarted.
Restart when the Unit is Hot and Sulfur is inside the Equipment
1. Start the incinerator (see Section 2.1).
2. Start the purge/ignition procedures for the main burner (see Section 2.1).
3. After establishing a stable natural gas flame, adjust substoichiometric
combustion at the main burner at a natural gas flow of 58 kg/h and air of 987
kg/h through the trim air line. Admit steam to the burner for cooling. The main
burner is now in the hot standby mode. Excess air should be avoided as it may
lead to sulfur fires.
4. It is assumed that the preheaters and reheaters are still in operation.
Adjust following temperatures:
Combustion chamber
Incinerator
1000 - 1300
240
750 - 800
C
C
C
5. Admit feed gas (see Section 2.3).
6.4.2
Restart when the Unit is Cold and Sulfur is inside the Equipment
1. Start the incinerator (see Section 2.1).
2. Start the purge/ignition procedures for the main burner (see Section 2.1).
3. After establishing a stable fuel gas flame, adjust the minimum design air flow of
987 kg/h through the trim air line and a fuel gas flow of 440 kg/h, corresponding
with 15% to 20% overstoichiometric combustion. Steam cooling is not allowed,
as it will condense on the cold walls of the downstream equipment. Only admit
steam to the burner when all equipment have reached a temperature of at least
80C.
When available, nitrogen can be supplied to the burner for cooling. Carefully
watch the temperature in the combustion chamber. In case the temperature
rises too rapidly, the burner should be stopped temporarily.
Watch the unit temperatures carefully. Be aware that sulfur fires may start, as
excess air is present. Ignition of FeS on the equipment walls might also occur.
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4. Start the reheaters. Slowly increase the temperatures of the reactor beds. The
Claus reactors temperatures should be restricted to 120C to avoid a sulfur fire
in the catalyst.
5. As soon as the equipment temperatures are above 80C steam can be supplied
to the main burner. Increase the natural gas flow to 58 kg/h to obtain
substoichiometric combustion. From now on, it is easier to have the
temperatures under control.
6. Continue with the heating-up procedure for the combustion chamber, incinerator
and reactor stages (see Section 2.1). The temperature rise in the combustion
chamber and incinerator is maximum 50C.
7. Adjust following temperatures:
Combustion chamber
Incinerator
1000 - 1300
240
750 - 800
C
C
C
8. Admit feed gas (see Section 2.3).
6.4.3
Restart when no Sulfur is inside the Equipment

When no sulfur is present in the unit, the normal startup procedure as described in
Section 5.4.1 can be followed.
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7.0
SAFETY
The following information deals with the prevention of possible dangerous situations
encountered in the Sulfur Recovery Unit.
7.1
AMBIENT H2S MONITOR EQUIPMENT

H2S is a very toxic gas. For protection of the operating personnel, an H2S monitor
system is installed.
The monitor is a multi-channel system specific for continuous monitoring of H2S in
the ambient air. The system consists of several local sensors and a common solid
state monitor. Each sensor has its own channel. The individual channels are
independent and each channel continuously reads the H2S gas concentration at its
remote sensor location. Manual override switching is included to permit a read out
of any given channel without interrupting automatic response of alarm circuits.
Meter range: 0 100 ppm vol. H2S.
The complete system consists of one monitor, local sensors, an indicator situated
on the control room panel and a warning alarm system in the unit as well as in the
control room.
The alarm is audible and visible.
When the concentration of H2S in the atmosphere, after the alarm is actuated,
appears to increase considerably, the unit has to be shutdown manually to stop all
incoming streams.
The alarm is set at a value of 25 (10) ppm vol. H2S.
It is advised to check the sensors every six months.
Process gas leaks of minor nature can be detected by means of cotton waste
soaked in ammonia. If this is brought into the vicinity of the leak, white fumes of
ammonium salts will be formed. In addition, filter paper wetted with lead acetate
solution can be used. The lead acetate turns black when exposed to H2S.
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7.2
SPECIAL SAFETY MEASURES AND INDUSTRIAL HYGIENE

This Section describes how to prevent hydrogen sulfide and sulfur dioxide
poisoning and some suitable protecting equipment.
Show responsible behavior
Carelessness, negligence or ignorance of danger are often the causes of H2S and
SO2 poisoning. Operators must be instructed to avoid inhalation of gas whenever
possible, by working on the windward side of the place where gas is escaping.
Furthermore, they should not stay unnecessarily without protection under process
gas lines or equipment, since H2S and SO2 are gases heavier than air.
Process staff and senior operating personnel have an additional responsibility and
they should show by their own example that precautions should be taken.
Instructive bulletins issued by the safety department and education are also very
important.
Personnel protection
a. Compressed air breathing apparatus/hose masks
In places where high concentrations of gas may occur, especially in enclosed
spaces, one should wear a compressed air breathing apparatus or hose masks
connected to a clean air supply. If an air blower supplies air, care must be taken
that the air blower has been placed upwind and clear of any source of gas, in
order that the person wearing the mask will have a supply of uncontaminated air.
When the aforementioned masks are in use an attendant should be stationed at
the air supply point. As an extra precaution somebody equipped with a
compressed air breathing apparatus should watch each hose and safety line and
prevent them from becoming entangled.
Even at low concentrations of H2S and SO2 a canister type mask may not be
worn, as this type is unreliable!
When loading or unloading catalyst, wearing of masks is recommended to
prevent inhalation of catalyst dust.
b. Life line
Personnel should not enter an enclosed space without a belt with a life line. In
addition, an attendant should remain in a safe location at the other end of the life
line at all times.
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c. Eye protection
To prevent irritation of the eyes full goggles with water dams are recommended.
The water dams prevent fogging of the lenses, which should be made of safety
glass.
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7.3
FIRST AID MEASURES

If a person has lost consciousness by inhalation of H2S or SO2 gas, the following
procedure is advised:
1. Remove the patient to fresh air or a well ventilated room and loosen any
restrictive clothing.
2. In conjunction with 1 above, contact the medical department, and call
immediately a doctor, stressing the nature of the accident.
3. Only a person familiar with the use of oxygen inhalation apparatus should carry
out application of oxygen to a patient. An attempt to apply oxygen by a person
not familiar with the use of the apparatus may result in the loss of valuable time
and may harm the patient.
4. Keep the patient comfortably warm, but not hot.
If the patient regains consciousness during this period, keep him as calm as
possible as he might be in a state of shock.
5. If, however, respiration of the patient has stopped, commence artificial
respiration treatment at once and continue until professional assistance arrives.
6. It should not be attempted to give anything to eat or to drink to an unconscious
patient.
Remark
Do not attempt to enter a gaseous area to render assistance before putting on a
compressed air breathing apparatus or air hose mask.
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7.4
TOXICOLOGICAL DATA
Tables of H2S and SO2 effects are given below, followed by a summary of some of
their properties.
7.4.1
Physiological Effects of H2S

ppm1) vol.
Effect
vol.%
1.
Limit for odor detection
0.14
2.
Weak odor hardly noticeable
0.77
3.
Noticeable odor
4.6
4.
Obnoxious odor
7.0
5.
MAC2)
10
0.001
6.
50 - 100
0.005 - 0.010
78 - 128
0.008 - 0.013
170 - 255
0.017 - 0.026
198 - 283
0.020 - 0.028
200 - 300
0.02 - 0.03
11.
Slight signs of inflammation of the eyes after one hour

Limit that can be stood for six hours without adverse
effects
Limit that can be stood for one hour without
consequences
Odour no longer disagreeable
Distinct signs of inflammation of the eyes after one
hour
Danger to life within thirty to sixty minutes
355 - 496
0.036 - 0.050
12.
Fatal within thirty to sixty minutes
425 - 580
0.043 - 0.058
13.
Fatal after half an hour
500 - 700
0.05 - 0.07
14.
Causing immediate fainting
700 - 1000
0.07 - 0.10
7.
8.
9.
10.
15. Immediately fatal

850 - 1980
ppm
= volume parts of H2S per million parts of air
1 ppm= 1 cm3/m3
2)
MAC = Maximum allowable concentration for an eight hours working day
0.085 - 0.2
1)
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7.4.2
Physiological Effects of SO2

ppm 1) vol.
Effect
Limit for odour detection

3-5
MAC 2)
5
Smallest amount causing immediate irritation of
3.
20
the eyes and throat
Maximum allowable concentration for
4.
50 - 100
30 - 60 minutes
5. Danger even with short exposure
more than 400
1)
ppm
= volume parts of H2S per million parts of air
1 ppm= 1 cm3/m3
2) MAC = Maximum allowable concentration for an eight hours working day
vol.%
1.
2.
7.4.3
0.002
0.005 - 0.010
0.040
H2S Properties and Toxic Effects

H2S is a colourless, inflammable and very toxic gas having an offensive odour and
sweetish taste. It has a specific gravity 1.17 times that of air.
The offensive odour, like that of rotten eggs, is not reliable as a warning of
dangerous concentrations, as persons differ greatly in the ability to detect smells,
and furthermore the sense of smell deteriorates and is of little help in noting higher
increased concentrations.
H2S is almost as toxic as hydrogen cyanide and six times as toxic as carbon
monoxide. The toxic effects vary considerably with the concentration and also to
some extent with individual susceptibility.
At low concentrations, it has an irritant action on the respiratory tract, which could
result in sickness, vomiting and a feeling of pressure on the chest. Simultaneously it
affects the nervous system.
At high concentrations, H2S paralyses the nervous system. Consequently the
respiration fails and death will follow immediately by suffocation. Even at low
concentrations, H2S affects the cornea of the eye.
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7.4.4
SO2 Properties and Toxic Effects

Sulfur dioxide is a colourless gas, with a specific gravity 2.2 times that of air.
In the presence of mist or water, this gas forms sulfurous acid.
The gas has a sour taste. It irritates the respiratory tracts because it forms, with the
water present, sulfurous acid and further sulfuric acid. This acid etches the human
tissue.
At low concentrations, it irritates the mucous membranes. Inhalation of higher
concentrations causes hoarseness, pain and a feeling of pressure on the chest and
bronchitis. It is sometimes impossible to speak or to swallow.
Very high concentrations cause acute bronchitis, tightness of the chest and a quick
start of perturbation of consciousness. Instant death by poisoning seldom occurs.
Suffocation, however, can cause death quickly. SO2 also causes an increase of
haemoglobin in the blood. The toxic effects vary to some extent with individual
susceptibility.
A certain immunization to SO2 is possible, to a maximum of 30 to 50 ppm vol.
Human beings can withstand a maximum of 20 ppm vol. without adverse effects.
Higher concentrations can give the victim a pale appearance, cause an unpleasant
taste in the mouth and can even make the gustatory nerves insensitive. Additional
effects are loss of appetite and constipation.
7.4.5
Sulfur Dust
Sulfur dust in the atmosphere has a highly irritating effect upon the human eye.
Therefore, safety goggles should be worn when working in an atmosphere where
dust contaminates the air. This cannot be overemphasized.
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7.5
FIRE AND EXPLOSIVITY DATA

H2S
The lower and upper limits for inflammability in a gas air mixture are 4.3 and
45.5 vol.%, respectively. In the stoichiometric ratio with oxygen, it explodes violently
when ignited. It is therefore necessary to handle hydrogen sulfide by excluding all
sources of ignition, open flames, sparks (including static discharges) and heat
producing equipment from contact with this gas when mixed with air. The autoignition of H2S in air will occur at a temperature of approximately 260C.
SO2
This is a non-inflammable gas.
Sulfur liquid
At a temperature of approximately 230C, auto-ignition of liquid sulfur will occur
when in contact with air. Therefore, attention must be paid to ensure that the liquid
sulfur temperature is maintained below the above-mentioned value. Ignition of the
sulfur will also occur when exposed in the area of an open flame, resulting in the
formation of SO2.
Sulfur dust
As stated above, liquid sulfur has a relatively low ignition point, 230C; however,
sulfur dust clouds will already ignite at a temperature of approximately 190C.
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8.0
8.1
TROUBLE SHOOTING
INTRODUCTION
The aim of this section is to draw the attention of operating personnel to some
undesirable conditions which may arise during otherwise normal operation and to
the means to prevent or remedy them. For other conditions not normally
encountered, see Section 6.5 ("Automatic Shutdown").
The operating problems in a sulfur recovery plant can be categorized into process
and mechanical problems. The process problems and operational hazards are
related to the sulfur recover unit such as poor sulfur recovery, pressure drop
problems, sulfur plugging and temperature runaways are discussed in this Section.
Mechanical problems which can occur are related to the bearings of running
equipment, ignition of burners, boiler leakage, refractory material and corrosion.
8.2
8.2.1
PROCESS PROBLEMS
General
a. Sudden temperature changes should be avoided whenever possible, since they
might cause leaks at flanges or loosening of iron sulfide scale from the
equipment walls.
b. During startup the acid gas shall not be burnt with too much air. It would result
in high flame temperatures that could damage the lining of the combustion
chamber and the tube plate of the waste heat boiler, if they are subjected to this
condition during a prolonged period of time. Moreover, the SO2 emission from
the stack would be excessively high.
c.
H2S and SO2 are extremely poisonous gases. Utmost care must be taken to
avoid exposure of personnel and environment to these gases, e.g. when
draining H2S containing liquid or when taking gas samples.
In special circumstances, protective masks must be worn (see Section 7).
d. The lower and upper explosion limits of H2S in a gas air mixture are 4.3 and
45.5 vol.%, respectively. In the stoichiometric ratio with air, it explodes violently
when ignited.
e. At a temperature of approximately 230C, auto-ignition of liquid sulfur will occur
when in contact with air. Sulfur dust will ignite at approximately 190C.
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f.
The waste heat boilers and condensers need to be checked regularly for the
boiler water quality. For this purpose, use the sample cooler to retrieve the
sample. In view of deposits in the sample lines and for the sake of good
sampling, flush the sample line at least for 10 minutes before taking a sample.
The maximum allowable total concentration of solids in the waste heat boiler is
3000 ppm, of which a maximum 250 ppm of suspended solids is permitted. The
maximum allowable total concentration of solids in the sulfur condensers is
3500 ppm with maximum 300 ppm of suspended solids.
Higher figures might lead to dirt and scale deposition and finally to damage of
the boiler and condensers. The concentration of solids can be adjusted by
varying the blowdown rate.
g. All steam traps should be checked frequently to ensure a proper heating

performance. In this way plugging of the process lines, equipment and valves
by solid sulfur can be avoided.
h. A frequent inspection of the sulfur flow from the sulfur locks and the flame color
as well as reading of the main burner inlet pressure may give an early warning
before plugging by sulfur and/or ammonia salts might occur.
i.
8.2.2
By a high unit pressure alarm the operator can first shutdown the SWS feed gas
supplies. In this way the unit throughput is reduced and the unit pressure will
decrease.
Burner & Combustion Chambers

a. Care should be taken that the air - to - natural gas ratio at the burner is correct.
A major deficiency of air at natural gas firing might result in deposition of soot
on the catalyst bed (higher pressure drop and less sulfur conversion). When the
unit is still hot, an air excess might result in equipment damage due to fire
inside the equipment. It might also cause sulfation of the Claus catalyst in the
second reactor, resulting in less sulfur conversion.
Soot can only be removed during a shutdown period by replacing the top layer
of the catalyst bed.
b. To prevent damage of the burner, it is strongly advised to operate the air side of
the burner at a pressure drop of at least 0.0015 kg/cm2.
c.
During the (natural gas) ignition stage in the main burner, the maximum amount
of natural gas allowed to be present inside the burner/combustion chamber is
restricted to avoid an excessive pressure rise when the actual ignition takes
place. For this reason the burner/combustion chamber are purged before
admitting natural gas to remove any combustibles that might be left from a
previous ignition trial.
The equipment is capable to stay leaktight after a pressure rise during ignition
or explosion, but the internals may be damaged.
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d. No carry-over of liquid hydrocarbons or high amounts of gaseous hydrocarbons

from preceding units should take place as it might damage the main burner/
combustion chamber. It might also cause soot deposition inside the unit, e.g. on
the catalyst beds.
e. The windows of the flame scanners and the pyrometer should be cleaned on a
regular basis.
f.
8.2.3
The temperature in the combustion chamber should be at least 1250C in order

to burn all of the ammonia during acid gas firing. If no ammonia is present, the
temperature should be at least 930C in order to have a stable flame.
Therefore, the steam tracing of the acid gas feed pipe should always be correct.
If this temperature is not reached, natural gas has to be supplied to the main
burner.
Reactor Stages
a. Runaway temperatures in the Claus reactors should be avoided during hot
standby and shutdown. When the temperature tends to rise to 350C the air - to
natural/acid gas ratio at the main burner should be reduced in order to obtain
substoichiometric conditions, and/or nitrogen can be introduced. Introduce 5 LP
Steam to the reactor for additional cooling (see also section 8.2.9).
b. Care should be taken that the ratio fuel gas-air at the main burner is correct.
Too little air might result in deposition of soot on the catalyst bed (higher
pressure drop and less sulfur conversion) and too much air in sulfation of the
catalyst (less sulfur conversion).
Soot, however, can only be removed during a shutdown period by replacing the
top layer of the catalyst bed.
c.
8.2.4
The performance of the tail gas analyzer should be checked regularly.
Incinerator
a. The incinerator is started-up before the main burner to convert any hazardous
gas, which might leave the unit during the purging and ignition phases of the
main burner.
b. To prevent damage of the burner, it is strongly advised to operate the air side of
the burner at a pressure drop of at least 1.2 mbar.
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8.2.5

a. Too high a liquid sulfur temperature should be avoided. Above 155C the
viscosity of the sulfur rises rapidly and may harm the sulfur pumps. Therefore,
the steam coils should only be in operation when no sulfur is produced in the
unit, unless the sulfur temperature drops below 125C.
b. In case the stripping has not been in operation for 7 hours the operator has to
trip the SRU, as an unsafe situation can occur at sulfur handling because the
H2S content in the liquid sulfur increases.
8.2.6
Poor Sulfur Recovery

a. A decrease of sulfur recovery is often caused by deactivation of the catalyst due
to sulfation. Sulfates are mainly formed by excess oxygen during shutdown
operation. Therefore, immediately after restart, the catalyst should be
reactivated. Also, if required, the catalyst can be reactivated during operation.
Reactivation (also called regeneration or rejuvenation) is the reduction of
sulfates at elevated temperature (as high as possible) with slight excess of H2S
at 2 - 3 vol.% (see Section 3.1.1).
Titanium catalyst (CRS-31) which is installed in the 1st Claus reactor is
insensitive to sulfation.
b. Catalyst deactivation can also occur when the reactor bed temperature drops
below the sulfur dew point of the process gas. This can be solved by raising the
reactor inlet temperature to 30C above the normal value for some time to
vaporize the sulfur (heat soak).
c.
Another cause of low sulfur recovery can be a poor acid gas/air ratio control. In
refineries, often the acid gas composition is not known and usually it fluctuates
during operation. The H2S/SO2 analyser corrects for this, but it is advised to
adapt the air/acid gas ratio if there is a continuous correction by the analyzer.
d. Good sulfur separation after each condenser is also important. For this
purpose, all sulfur condenser outlet channels have been provided with demister
pads. Furthermore, a coalescer with demister downstream the last condenser
has been provided.
e. In the main burner, COS and CS2 are formed as by-products. They are present
especially when large amounts of CO2 and/or hydrocarbons are present in the
feed gas. If they pass through the unit untouched, they account for some loss of
sulfur recovery. However, at a sufficiently high temperature (higher than 300C),
COS and CS2 are largely hydrolyzed to H2S in the first Claus reactor. Therefore
it is important to maintain the 1st reactor outlet temperature above 300C.
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8.2.7
Pressure Drop
Soot, corrosion products such as FeS or refractory fines or ammonium salts can be
the cause of an increasing pressure drop over the unit.
Soot is formed when hydrocarbon carry-over from the amine regeneration units
occur. The flow ratio controller cannot follow such upsets, and hydrocarbons are
carried through the whole unit and too little H2S is burnt in the main burner.
Sometimes a fire starts in the incinerator and/or stack due to combustion of large
quantities of H2S.
Soot is deposited on the catalyst and the sulfur produced is brown or black under
such conditions. Hydrocarbon carry-over can be prevented by better operation
and/or modifications to the amine regeneration units.
Another possibility of soot formation occurs when the burners are fired at very low
air/natural gas ratios. It is recommended to keep the ratio at 90 - 95% stoichiometry.
This can be checked visually by observing the color of the flame, which should be
salmon pink when natural gas is fired. Always stay above 80% stoichiometry to
prevent soot formation.
A common refinery regeneration procedure to remove soot is to burn off the soot at
500C flame front temperature. This procedure, however, is not recommended as
this high temperature will promote sulfur fires and sintering of the catalyst. Jacobs
Nederland B.V. policy is to replace 10 cm top layer of the catalyst as standard
procedure at each turn-around or at shutdown caused by too high pressure drop.
Sulfur demisters may be plugged by sulfur. Therefore, all demisters have been
located in an outlet channel provided with a steam tracing to keep the outlet
channel hot. The demisters can easily be removed through the drawers.
The pressure drop in a sulfur recovery unit is proportional to the square of the
throughput. Operators should daily check the plant pressure drop to make sure they
notice early warnings in case the pressure drop starts to deviate. To simplify their
work the pressure drop can be said to be proportional to the square of the air flow.
As the pressure drop, divided by the square of the air flow, should be a constant
figure, early warning of pressure drop problems can be found by daily plotting this
ratio.
8.2.8
Plugging
Sulfur plugging
Sulfur plugging problems are usually experienced in sulfur lines and sulfur locks.
When plugging is caused by pure solid sulfur, for example due to a malfunctioning
steam trap, is easily removed by heating. Sulfur, however, in combination with
corrosion products, refractory and/or catalyst fines may give grey sulfur (concrete
sulfur) which is difficult to remove. At initial startup the catalyst beds should be air
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blown to remove fines (see Section 4.5). Careful cleaning of the tubes of waste heat
boiler, sulfur condensers, sulfur lines and sulfur locks will eliminate plugging
problems at startup.
Plugging of sulfur locks

Plugging of sulfur locks or sulfur rundown lines can be detected by checking the
funnels. Please note that personnel protection should be used, see also section 7.2.
The system is plugged when no liquid sulfur flows. When a sulfur lock is plugged,
an LP steam or nitrogen hose can be connected to the top of the lock. The block
valve in the sulfur rundown line is closed and the lock is blown with the steam or
nitrogen. If plugging occurs in the sulfur rundown line, the sulfur lock outlet is to be
blinded off. Then lock and sulfur lines are blown in the direction reverse to normal
flow. At other locations, remove the jacketed elbows in order to blow through.
Especially the sulfur locks downstream the Claus condenser and the coalescer shall
be checked regularly at least on a daily basis. Because of the relatively low
temperature, the danger of plugging is here higher.
Ammonia salt plugging
During considerable upsets in the SWS gas (excess NH3) or hydrocarbon carry over
from the Amine Regeneration Units, there may be temporary deficient of air. Under
these circumstances the possibility exists that the ammonia is not converted
completely. If so, ammonium salts are formed. Also when burning ammonia in a
Claus plant below the temperature limit of 1250C, ammonium salts are formed.
These salts are experienced at the locations of the lowest temperature in the plant
like outlet channels of the condensers, wire demisters, sulfur lines and locks
resulting in pressure drop problems.
In particular ammonium salts are formed at the outlet of the final condenser and
coalescer where the salts tend to plug the mist mats. Fortunately the formation is
reversible and at a temperature of 150C or above the salts sublimate into the
process gas. In order to achieve this temperature, the steam pressure in the final
condenser can be increased to 3.2 kg/cm2g. In addition, the flame temperature is to
be raised above 1250C by using the preheaters and/or co-firing natural gas (if
necessary).
8.2.9
Temperature Runaways
Fire inside the Claus reactors
During the shutdown phase and hot standby operation a rapid temperature rise in
one of the catalyst beds (temperature runaway) may occur when too much air is
supplied to the main burner. Then the sulfur, absorbed in the catalyst, reacts
violently with the oxygen in the air, resulting in a fire. A fire inside the reactor bed
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deactivates the catalyst by severe sulfation and sintering. Shut-down procedures,

as described in section 6.0 will prevent these temperature runaways.
When a temperature runaway happens, the air supply to the main burner should be
decreased and/or the natural gas supply should be increased to stop the air breakthrough from the burner. The corresponding steam reheater should be stopped by
adjusting the setpoint of the temperature controller. LP steam should be introduced
directly into the reactor. When the temperature is dropped, the steam reheater can
be restarted.
Also, sulfur elsewhere in the plant can be set on fire by uncontrolled amounts of
oxygen. In a sulfur plant design, dead spots where sulfur may accumulate should
be prevented. All equipment in which sulfur condenses, should have a proper slope.
Fire in the sulfur pit
Fire inside a sulfur pit is often caused by static electricity. A fire in the sulfur pit is
detected by the temperature alarm in the air space of the sulfur pit. The fire should
be extinguished by injection of smothering steam.
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8.3
MECHANICAL PROBLEMS
8.3.1
Running Equipment
Problems with running equipment mainly concern bearings. The engineering
companies and manufacturers should pay proper attention to the bearing design to
prevent those problems. Sulfur pump bearings, for example, should have a
clearance of 0.6 mm and heating steam may not exceed 160oC because sulfur
viscosity rapidly rises above 155C, especially when degassed sulfur is pumped.
8.3.2
Ignitors
The main problems are ignition difficulties and damage to the ignitor tip by
overheating if they are not withdrawn properly after ignition. Ignition problems are
often caused by short circulating due to moisture. Another cause can be excessive
back pressure in the burner chamber, in combination with an inert gas atmosphere.
Overheating of the ignitor connection can be prevented by adequate
cooling/purging with either air or inert gas.
8.3.3
Boiler or Condenser Leakage

Although these problems seldom occur, it is difficult to distinguish the symptoms. A
decrease of steam production, a lower gas outlet temperature of the boiler and a
higher plant pressure drop are the first indications. A method to determine whether
there is a leakage is to stop the blow down of boiler water and to analyze the
phosphate and salt content of the water in the boiler or condenser. If a leakage is
identified, the plant should be stopped to prevent a crash shutdown.
8.3.4
Refractory Material
Selection and correct installation of refractory material in Claus plants is important
to prevent cracking and collapse. Experience has shown that refractory lining for the
main combustion chamber should be made of brick. Concrete lining for these high
temperature applications gives disappointing results because of the difficulty of
making a homogeneous mixture when it is installed. Radiation walls, on the other
end, should preferably not be made of brick but of castable matrix blocks, fitted
together without using mortar. The advantage of such walls is that they can be
easily removed and reinstalled at turnarounds.
Refractory lining of the waste heat boiler tube sheet should be made of castable
material, such as (with a high Al2O3 content, >94%), in combination with ceramic
ferrules. The hot gas part of the incinerator should be made of bricks, refractory
linings of the incinerator can be made of castable material.
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8.3.5
Fluctuations and Hydrocarbon carry-over

Refinery Claus plants compared to natural gas Claus plants are often confronted
with hydrocarbon carry-over and feed gas fluctuations. An H2S tail gas analyzer, as
part of the acid gas/air ratio control system will correct the ratio as long as the
fluctuations are within certain limits. Claus plants without an H2S/SO2 tail gas
analyzer are more or less blindly operated. Operators will notice a change in
quantity but will not be able to observe any change in gas composition.
A problem is the carry-over of hydrocarbons. The acid gas/air ratio control cannot
follow such upsets, even if a tail gas analyzer is available, and all kinds of operation
problems (temperature runaways, soot, plugging) may be the result. As soon as the
Claus plant has to be shut down because of operating problems, the acid gas has
to be flared and another problem arises: high SO2 emission.
In refineries in which spare Claus plant capacity is available, operators have the
possibility to operate both plants simultaneously or one on hot stand-by. Upsets in
the Claus feed gas when both plants are simultaneously operated will affect both
units and will have to deal with two problems at the same time. When one unit is on
hot stand-by, it takes time and operating manpower to put the unit on stream.
During this period there is also an SO2 emission problem.
The installation of solvent buffer vessels in the upstream gas treating unit will solve
the problems. Moreover, flaring of acid gas during shutdowns can be prevented.
Buffer vessels improve the separation of hydrocarbons from the solvent and restrict
feed gas fluctuation.
8.3.6
Corrosion
Corrosion in Claus plants during normal operation is limited, if the related piping is
adequately steam heated and properly insulated. Severe corrosion may take place
when a Claus plant is out of operation for longer periods and the plant is
insufficiently purged and dried with inert gas. Corrosion is then caused by H2O, O2,
SO2 and CO2. Proper shutdown procedures and purging with a dry inert gas will
avoid severe corrosion problems. Leakage of acid gases to atmosphere has to be
prevented to avoid outside corrosion. Steel parts in the sulfur collecting pit are
sensitive to corrosion.
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8.4
CRITICAL AREAS IN SULFUR RECOVERY PLANT OPERATION

MAIN CAUSES
PHENOMENON OBSERVED
COUNTERMEASURES IN
DESIGN/OPERATION
1. MAIN COMBUSTION CHAMBER

a.
Damage of the burner gun of Main

Burner due to heat attack (especially
during startup, low load and
shutdown operation).
Poor combustion of acid gas with

combustion air.
Selection of Main Burner with adequate

pressure drop in all operational ranges.
Increase in residual NH3 content

increase in SO3 formation
increase in residual O2 content.
Management on pressure drop indicator

installed on combustion air side
(Operation above limitation:
> 0.0015 kg/cm2).
(Above phenomena resulting in plugging

and/or corrosion in downstream
equipment/lines).
b.
Damage of refractory lining due to

exceeding maximum service
temperature (flame direct contact) or
anchor failure initiated by hot gas
soaking.
Hot shell/hot spot (shutdown).
Management on temperature indicators

installed on Main Combustion Chamber.
Steam injection S atomizing flame.
Adjustment in upstream gas treating unit
(S).
Application of homogeneous mixing
especially for nozzles of sight gas pilot
burner and instrument connections.
c.
Internal explosion (especially during

startup and shutdown).
2.
WASTE HEAT BOILER
a.
Failure of tube-tube sheet joint due to

high temperature sulfide corrosion in
process gas side.
Leakage is of highly toxic nature (H2S)

(shutdown).
Application of explosion proof equipment

(explosion pressure).
Leakage of boiler feed water (shutdown).
Adequate maintenance for ferrules in tube

and lining of tube sheet.
Application of adequate tube sheet
thickness.
Application of strength welding or J-bevel
welding with adequate expansion for
tube-tube sheet joint.
b.
Rupture of tube due to erosion and

corrosion.
Leakage of boiler feed water (shutdown).
Management on quality of boiler feed

water.
Adequate tube arrangement.
c.
Internal explosion especially during

startup and shutdown.
Leakage is of highly toxic nature (H2S)

(shutdown).
Application of explosion proof equipment

(explosion pressure for inlet tube sheet
and outlet channel).
d.
Plugging of sulfur and/or ammonium

salt (in case of LP steam production).
High pressure drop (shutdown).
Selection of moderate operating

temperatures.
Increase in gas outlet temperature by
increasing product steam level.
Adjust Main Burner operation (minimizing
residual NH3 and preventing SO3
formation).
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MAIN CAUSES
3.
REACTORS
a.
Accumulation of soot.
PHENOMENON OBSERVED
COUNTERMEASURES IN
DESIGN/OPERATION
High pressure drop and black sulfur

production (regeneration or skimming
during shutdown).
Correction of natural gas/air ratio in case

of heavy fluctuation in the natural gas
composition.
b. Sulfation.
Poor sulfur recovery

(catalyst regeneration during low load or
before shutdown).
Application of special catalyst to prevent

sulfation.
Adjust Main Burner operation (minimizing
residual NH3 and preventing SO3
formation).
Correction of natural gas/air ratio for
preventing free O2.
c. Temperature runaway.
(Claus reactors)
Poor sulfur recovery

(Sieving damaged catalyst or replace with
new one).
Control for preventing O2 injection through

main burner.
Application of snuffing steam system in
each Claus reactor inlet line.
d.
Plugging of sulfur with other

contaminants.
High pressure drop.

(Adjustment of operation condition).
Increase in reactor inlet temperature.

Application of 50 mm insulation on
reactors to minimize heat loss.
e.
Liquid sulfur formation on catalyst.
Poor sulfur recovery (catalyst heat soak).
Increase in reactor inlet temperature with

approximately 30C.
4.
REHEATERS
a.
Rupture of tube due to erosion and

corrosion
High pressure at process side due to

steam leakage (shutdown)
Adequate tube material (stainless steel)
5.
SULFUR CONDENSERS
a.
Plugging of sulfur and/or ammonium

salt in tube and demister.
High pressure drop (shutdown).
Selection of moderate operating

temperature (above melting point)
increasing product steam pressure.
Adjust Main Burner operation
b.
Corrosion in outlet channel due to

SO3 condensation.
Leakage of boiler water (shutdown).
Selection of moderate operation

temperature (above dewpoint of SO3).
increasing product steam pressure
Adjust Main Burner operation.
6.
SULFUR DEGASSING VESSEL
a.
Internal explosion due to H2S content

in vapor space above liquid sulfur in
vessel (low explosion limit:
approximately 4 vol.%).
Damage of equipment installed in vessel

and fire of product sulfur.
Adequate H2S sweeping.

Installation of flow meter in vent gas
line(s) with emergency system and/or online H2S analyzer with emergency system
- provision of snuffing steam system.
b.
Corrosion of steam coil due to H2S

and wet atmosphere.
Steam leakage.
Application of stainless steel pipe or

carbon steel pipe with enough thickness.
Keep dry condition during shutdown
period.
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MAIN CAUSES
PHENOMENON OBSERVED
c.
For degassing pit: corrosion of steel

between concrete walls as water shield, due to difference in thermal
expansion.
7.
LIQUID SULFUR LINE(S) AND

SULFUR SEAL(S)
a.
b.
COUNTERMEASURES IN
DESIGN/OPERATION
Damage of degassing pit concrete wall

and destruction of degassing pit.
Enough investigation on degassing pit

type selection in case that ground water
level is higher than degassing vessel pit
depth.
Application of plastic material as water
shield (4 layer construction).
Application of submerged carbon steel
tank with alumina coating.
Solid sulfur plugging due to

malfunctioning steam trap.
Pressure drop increase.
Management on steam supply conditions

and check on operation of steam trap(s)
by solid sulfur lump.
Plugging of sulfur with corrosion

products, refractory and/or catalyst
fines (concrete sulfur).
Pressure drop increase (replace with new

one).
Enough and careful cleaning before

startup (wire brush).
Provision of blowing facilities in line(s)
and seal(s) with air and steam.
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9.0
MAINTENANCE
9.1
EQUIPMENT
9.1.1
a.
b.
c.
d.
e.
f.
Knock-out Drums
Clean the inside of the knock out drum from loose scale and dirt.
Clean the demister mat with steam.
Pressure test the steam coil, which is at the outside of the drum.
Check the condition of the demister support.
Outlet nozzle at the bottom should be freed from dirt.
Check the condition and mounting of the gas inlet device.
9.1.2
Preheaters
a. Clean the shell side and tubes at the outside, in such a way that they are freed
from any loose scale and dirt.
b. Pressure test the steam side of the preheater for approx. 2 hours after cleaning
activities.
c. Check the steam traps.
9.1.3
Burners
a. Remove the burners from the equipment.
b. Check if the metal parts of the burners have not been damaged by overheating.
Measure the dimensions of the burner gun and air nose. If significant deviations
are observed LD Duiker, the burner manufacturer, should be contacted.
Attention should be given to the vanes of the air register, the burner gun and tip
and the air nose. Replace damaged parts.
c. Check the electric ignitor. The tip may have to be replaced.
d. Check the refractory lining on cracks.
e. Clean the burners, including sight glasses and flame detectors.
f. Clean the air chamber of the burners and check if the drains are clean.
9.1.4
Combustion Chambers
a. Check the refractory lining of the chamber, bricks which are not in correct
position have to be replaced. Castable refractory, which is damaged, should be
repaired.
b. Inspect if the matrix blocks of the protection wall are still in place. Replace those
matrix blocks which are cracked.
c. Replace the ceramic well of the temperature indicator (instrument department).
d. Clean the chamber from dust.
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9.1.5
Waste Heat Boiler

a. Check the lining of the connection to the main combustion chamber. Bricks
which are not in correct position have to be replaced.
b. Remove the lining and ferrules from the tube plate, in case of severe cracking.
Clean the tube plate and check for leaking tubes and tube welds. Leaking tubes
can be plugged off to maximum 5% of the total number of tubes. Leaking tube
welds should be repaired. Install new ferrules, with a 2 mm smaller diameter
than original ones and install new tube plate lining.
c. Tubes to be wire brushed inside and to be air blown, in such a way that they are
freed from any loose scale and dirt before new lining is applied.
d. Remove rust and scale from outlet channel.
e. Clean the waterside of the boiler. Special attention should be paid to the bottom
of the boiler and the blow down drain.
f. Pressure test the waterside of the boiler for approximately 2 hours after
cleaning activities.
g. Check the main steam valve.
h. Bank testing of the safety relief valves.
9.1.6
Sulfur Condensers
a. Remove rust and scale from the inlet channel. Check the condition of the lining
in the inlet channel. If the concrete surface is not flat, fill the holes with concrete
and smoothen surface. Clean the tube plate and check for leaking tubes and
tube welds. Leaking tubes can be plugged off to maximum 5% of the total
number of tubes per condenser. If the lowest row of tubes has to be plugged off,
install additional concrete layer in the inlet channel to prevent collection of
sulfur. Leaking tube welds should be repaired.
b. Tubes to be wire brushed and to be air blown inside, in such a way that they are
freed from any loose scale and dirt.
c. Remove rust and scale from the outlet channel. Sulfur outlet nozzle to be wire
brushed. Check the condition of the lining in the outlet channel. If the concrete
surface is not flat, fill the holes with concrete.
d. Check the condition of the wire mat. If the mat is fouled and cleaning is
impossible, the wire mat has to be replaced.
e. Pressure test the steam coil, which is installed below the demister.
f. Clean the waterside of the Claus condenser. Special attention should be paid to
the blow down drain nozzle.
g. Pressure test the water side of the Claus condenser for approximately 2 hours
after cleaning activities.
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9.1.7
Reactors
a. Open the top manholes of the reactors (catalyst should be protected during
rainfall).
b. Check the condition of the top layer of the catalyst. In case only the top layer is
soothed (black), the top 100 mm is replaced. If the catalyst is heavily soothed,
the recommended procedure for removing the soot is by screening. The
catalyst has to be taken out of the reactor. Never burn off carbon deposits.
c. Take catalyst samples from each reactor, halfway each catalyst layer. The
samples are sent to the catalyst manufacturer for analysis. Sampling of the
catalyst is advised some time prior to the maintenance shutdown.
d. Check the condition of the concrete lining as far as possible. If the refractory
material is dropped or loose from the cracks, which are usually present, the
refractory should be repaired.
e. Remove the expansion bellows from the gas outlet piping for cleaning and
examination of the bottom part of the reactor.
f. Check the condition of the support grid and gauze.
g. Check the expansion bellows.
h. Lock the expansion bellows before removing them.
i. Leak test the expansion bellows.
9.1.8
Sulfur Coalescer
a. Clean the inside of the coalescer from loose scale and dirt.
b. Check the condition of wire mat. If the mat is fouled and cleaning is impossible,
the wire mat has to be replaced.
c. Check the condition of the demister support.
d. Sulfur outlet nozzle to be wire brushed.
e. Check the condition and the mounting of the gas inlet device.
9.1.9
Incinerator
a. Check the condition of the concrete lining. If refractory material is dropped or
loose from the cracks, which are usually present, the refractory should be
repaired.
b. Clean the chamber from dust.
c. Check the air distributors for corrosion.
9.1.10
Incinerator Waste Heat Boiler

a. Check the lining of the connection to the thermal incinerator. If refractory
material is dropped or loose from the cracks, which are usually present, the
refractory should be repaired.
b. Remove the lining and ferrules from the tube plate, in case of severe cracking.
Clean the tube plate and check for leaking tubes and tube welds. Leaking
tubes can be plugged off to maximum 5% of the total number of tubes.
Leaking tube welds should be repaired. Install new ferruled, with a 2 mm
smaller diameter than the original ones and install new tube plate lining.
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c. Tubes to be wire brushed inside and to be air blown, in such a way that they
are freed from any loose scale and dirt before new lining is applied.
d. Remove rust and scale from outlet channel. Check the conditions of lining in
outlet channel and repair if required.
e. Clean the waterside of the boiler. Special attention should be paid to the
bottom of the boiler and the blow-down drain.
f. Pressure test the waterside of the boiler for approximately 2 hours after
cleaning activities.
g. Check the main steam valve.
i. Check the condition of the connection from the incinerator waste heat boiler to
the steam superheater. Check refractory lining and repair if required.
9.1.11
Steam Superheater
a. Clean the shell side and tubes at the outside, in such a way that they are
freed from any loose scale and dirt before new lining is applied.
b. Pressure test the steam side of the superheater for approximately 2 hours
after cleaning activities.
c. Check the steam traps.
d. Check the conditions of the flue duct from the steam superheater to the stack.
Check the flue duct lining and repair if required.
9.1.12
a.
b.
c.
d.
e.
f.
9.1.13
9.1.14
Sulfur Locks
Remove as much as possible the sulfur from the locks as follows:
- Close the valve in the sulfur rundown line.
- Connect steam or nitrogen hose on the utility connection of the sulfur lock.
- Admit steam or nitrogen to the sulfur lock, thereby removing sulfur from the
lock.
- Disconnect steam hose.
Remove the sulfur locks from their shafts.
Remove the bottom flange of the sulfur lock and clean the inside of the lock.
Pressure test the steam jacketing of the locks.
Check the valves.
Check the condition of funnels.
Sulfur Storage Tank
a. Sulfur storage tank should be pumped out and cleaned completely.
b. Inlet and outlet vent pipes to be wire brushed.
c. Pressure test the steam coil, which is at the outside of the sulfur storage tank.

a. Sulfur degassing vessel should be pumped out and cleaned completely.
b. Sulfur pumps should be removed and overhauled.
c. Bottom pumps to be cleaned.
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d. Inlet and outlet vent pipes to be wire brushed.

e. Check supports of the sulfur degassing vessel covers.
f. Check condition bubble columns, including baffles and air spargers.
9.1.15
Steam Coil in Sulfur Degassing Vessel

a. Wire brush the outside surface of the steam coils, including inlet and outlet
piping inside the sulfur degassing vessel.
b. Pressure test the steam coils in order to detect leaks. Leaking welds to be
repaired.
c. For maximum security, the condition of the welds can be checked by X-raying.
9.1.16
Running Equipment
a. For inspection and maintenance of all running equipment, reference is made to
the maintenance instruction manual of the manufacturers.
b. Suction screens of pumps and blowers to be cleaned and checked.
9.1.17
Piping and Valves

a. Wire brush all sulfur lines.
b. Wire brush the main process gas lines.
c. Steam out the propane gas lines. Remove and clean filters in these lines.
Replacement of filters may be required.
d. Lubricate and ease all valves.
e. Clean all steamtraps and lines.
f. Clean all restriction orifices in purge lines.
9.1.18
Analyzers
a. Clean sample valves and sample lines (with steam).
b. Clean internal of analyzers according to the manufacturers instructions
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ATTACHMENTS
SAFETY DATA SHEETS FOR CLAUS
CATALYST
Page 90 of 91
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Doc. no. 64566-13/P.02/0011/A4

Page 91 of 91
Rev. October 2006

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Doc. no. 64566-13/P.02/0011/A4

Operating & Maintenance Manual - SRU: Total, Lindsey Oil Refinery, Humberside, England

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