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Operating-Guidelines of Plant and LAB
Operating-Guidelines of Plant and LAB
SULFUR BLOCK
OPERATING GUIDELINES
Prepared by
Ortloff Engineers, Ltd.
Midland, Texas USA
Project 507000
Fall 2011
Operating Guidelines Samsung Total Petrochemicals Co., Ltd.
Fall 2011 Daesan, Korea
SULFUR BLOCK
Table of Contents
1. INTRODUCTION .......................................................................................................... 1-1
1. INTRODUCTION
These Operating Guidelines have been prepared by Ortloff Engineers, Ltd. as a guide
for the initial operation of the new Sulfur Block at Samsung Total Petrochemicals Co.,
Ltd.’s Daesan No. 2 Aromatics Complex. The new Sulfur Block consists of an Amine
Treating Unit (ATU), an Amine Regeneration Unit (ARU), a Sour Water Stripper
(SWS), two parallel Sulfur Recovery Units (SRUs), and a common Sulfur Degassing
Unit (SDU), Tailgas Cleanup Unit (TGCU) and Tailgas Thermal Oxidation Unit (TTO).
These units are to process sour gas and sour water streams to remove the contained
sulfur and produce treated fuel gas for consumption in the complex, treated water
safe for reuse or disposal, and commercial grade molten sulfur for sales. These
guidelines contain information concerning the design, startup, operation, and
shutdown of the new facility to assist plant personnel in developing familiarity with
and understanding of the process, equipment, and overall plant operation, and to
supplement equipment manufacturers' operating instructions.
1. Purpose of System
2. Safety
3. Process Description
6. Precommissioning Procedures
7. Startup Procedures
8. Shutdown Procedures
The instructions in these guidelines are based on past experience with similar plants
and equipment. They are to be used as guidelines for developing detailed operating
procedures customized for your plant and its actual operating conditions. These
instructions are not intended in any way to supersede or supplant operating
procedures and safety practices established by Samsung Total Petrochemicals Co.,
Ltd., nor are they intended to be used independently of equipment manufacturers’
operating instructions. In preparing these instructions, it has been assumed that all
startup and operating personnel have been trained in and are knowledgeable of the
operating instructions provided by the manufacturers of the equipment included in this
facility.
It is expected that Samsung Total Petrochemicals Co., Ltd. will revise and improve
upon the operating instructions in this manual as operating experience is gained, and
as required to incorporate any changes resulting from Samsung Total Petrochemicals
Co., Ltd.'s Process Safety Management program. Update and maintenance of this
manual is Samsung Total Petrochemicals Co., Ltd.'s responsibility and is not within
Ortloff's scope of responsibility.
Operating values and numbers quoted in this manual are design values. They are
presented to enable the operator to have a "ball park" idea of plant operating values.
Actual plant operating conditions may deviate from the design figures, yet yield
satisfactory operations and products. We recommend that operating parameters
such as temperatures, pressures, and flow rates be recorded on a routine basis.
Good data, properly gathered and maintained, form a valuable base for plant studies
and performance evaluations.
Table of Contents
2. GENERAL SAFETY ..................................................................................................... 2-1
2.1 DEFINITION OF TERMS ....................................................................................... 2-1
2.2 HYDROGEN SULFIDE (H2S) ................................................................................ 2-3
2.2.1 Description and Properties ............................................................................. 2-3
2.2.1.1 General.................................................................................................... 2-3
2.2.1.2 Toxicity Information ................................................................................. 2-3
2.2.1.3 Permissible Exposure Limits ................................................................... 2-3
2.2.1.4 Odor ........................................................................................................ 2-3
2.2.1.5 Physical Data .......................................................................................... 2-3
2.2.1.6 Reactivity Data ........................................................................................ 2-4
2.2.1.7 Corrosivity Data ....................................................................................... 2-5
2.2.1.8 Water Solubility ....................................................................................... 2-5
2.2.1.9 Other Characteristics............................................................................... 2-5
2.2.1.10 Fire and Explosion Hazard ...................................................................... 2-6
2.2.1.11 Life Hazard .............................................................................................. 2-6
2.2.2 First Aid .......................................................................................................... 2-7
2.2.3 Precautions (remember these facts) .............................................................. 2-8
2.2.4 Good Work Practices...................................................................................... 2-9
2.3 SULFUR DIOXIDE (SO2) ..................................................................................... 2-10
2.3.1 Description and Properties ........................................................................... 2-10
2.3.1.1 General.................................................................................................. 2-10
2.3.1.2 Toxicity Information ............................................................................... 2-10
2.3.1.3 Permissible Exposure Limits ................................................................. 2-10
2.3.1.4 Odor ...................................................................................................... 2-11
2.3.1.5 Physical Data ........................................................................................ 2-11
2.3.1.6 Reactivity Data ...................................................................................... 2-11
2.3.1.7 Corrosivity Data ..................................................................................... 2-12
2.3.1.8 Water Solubility ..................................................................................... 2-12
2.3.1.9 Fire and Explosion Hazard .................................................................... 2-12
2.3.1.10 Life Hazard ............................................................................................ 2-12
2.3.2 First Aid ........................................................................................................ 2-13
2.3.3 Precautions................................................................................................... 2-14
2.4 SULFUR .............................................................................................................. 2-15
2.4.1 Description and Properties ........................................................................... 2-15
2.4.1.1 General.................................................................................................. 2-15
2.4.1.2 Toxicity Information ............................................................................... 2-15
2.4.1.3 Permissible Exposure Limits ................................................................. 2-15
B. Sulfur Dioxide
C. Sulfur
D. Ammonia
E. Methyldiethanolamine
F. Sodium Hydroxide
2. GENERAL SAFETY
General
The safety information published herein is for guidance only and is not intended to
supersede or replace your company's safety procedures program where a conflict of
terminology or procedure may exist.
Safety Considerations
C. Flash Point
Specific gravity of solids and liquids is the ratio of the weight of any solid
or liquid to the weight of an equal volume of water. Therefore, if the
specific gravity of a substance is a number less than one, it is lighter than
water, and if the number is greater than one, it is heavier than water.
Specific gravity of gases is the ratio of weight of any gas to the weight of
an equal volume of air. Therefore, if the specific gravity of a gas is a
number less than one, it is lighter than air, and if the number is greater
than one, it is heavier than air.
F. Specific Volume
G. Toxicity
2.2.1.4 Odor
In low concentrations, H2S smells like rotten eggs. Higher
concentrations quickly damage the ability to smell and cannot be
detected by the characteristic rotten egg odor.
Formula Name
C2H4O acetaldehyde
BaO + Hg2O + air barium oxide + mercury oxide in air
BaO + NiO + air barium oxide + nickel monoxide in air
BaO2 barium peroxide
BrF5 bromine pentafluoride
C6H4BrN2Cl p-bromobenzene diazonium chloride
ClO chlorine monoxide
ClF3 chlorine trifluoride
CrO3 chromium trioxide (chromic anhydride, chromic
acid)
Cu copper
Fe2O3·nH2O di-iron trioxide hydrate
F2 fluorine
hydrated iron oxide
PbO2 lead dioxide (lead peroxide)
metal oxides
metals
HNO3 nitric acid
NCl3 nitrogen trichloride
NF3 nitrogen trifluoride
NI3 nitrogen triiodide
oxidizing materials
OF2 oxygen difluoride
ClO3F perchloryl fluoride
C6H5N2Cl phenyl diazonium chloride
rust
Ag2C2N2O2 silver fulminate
NaOH + CaO soda lime (a mixture of sodium hydroxide and
calcium oxide)
Na sodium
NaOH + CaO + air sodium hydroxide + calcium oxide (lime) in air
Na2O2 sodium peroxide
The following table from the U.S. Bureau of Mines represents the
degree of inhalation hazard with varying concentrations of hydrogen
sulfide:
Fatal in exposures of thirty minutes or less 600 & above 0.06 & above
For severe irritation of the eyes, hold the lids open and pour clean water
over the eyeball and lids (or use an eye irrigation fountain). Wash
thoroughly in this fashion for 15 minutes. A physician, preferably an eye
specialist, should be summoned immediately.
b. In the rich and lean amine streams in the Amine Treating Unit.
f. In the amine acid gas, the TGCU recycle gas, and the SWS gas
(the feed gases for the Sulfur Recovery Unit).
1. Make adequate plans to cope with any situation that may develop.
3. Observe the wind direction. Stay upwind if possible and warn others
who may be downwind.
2.3.1.4 Odor
Sulfur dioxide has a pungent, suffocating odor that can be detected
at very low concentrations, 0.3 to 1.0 PPM, possibly by taste rather
than odor.
Formula Name
C3H4O acrolein
Al aluminum
CsHC2 cesium hydrogencarbide
Cs2O cesium oxide
x-ClO3 chlorates
ClF3 chlorine trifluoride
Cr chromium
FeO ferrous oxide
F2 fluorine
lithium acetylene carbide diammino
Mn manganese
KHC2 potassium carbide
KClO3 potassium chlorate
Rb2C2 rubidium carbide
Na sodium
Na2C2 sodium carbide
SnO tin monoxide
Formula Name
halogens or interhalogens
LiNO3 lithium nitrate
x-C2H metal acetylides
metal oxides
metals
polymeric tubing
NaH sodium hydride
SO2 chiefly affects the upper respiratory tract and the bronchi. It may
cause edema of the lungs or glottis, and can produce respiratory
paralysis. (Edema is a condition in which irritated tissues swell,
collect fluid, and slowly excrete a watery fluid, in this case into the
lungs or voice box.)
If there are no signs of lung congestion at the end of this period, and if the
breathing is easy and the color is good, oxygen inhalation may be
discontinued. Throughout this time, the patient should be kept
comfortably warm, but not hot.
For irritation of the eyes, flush them with large amounts of warm water for
at least 15 minutes. It is advisable to irrigate the eyes gently with water at
room temperature in order to minimize additional pain and discomfort.
Take the patient to a physician, preferably an eye specialist, at once.
2.3.3 Precautions
Special precautions should be observed when fighting sulfur fires. Sulfur
fires should be approached from an upwind direction if possible, and
respiratory equipment should be used in the case of larger fires or when
fires are in enclosed areas. SO2 is always present in the following
locations:
2.4 Sulfur
2.4.1 Description and Properties
2.4.1.1 General
Sulfur is a yellow solid at normal ambient temperatures. However, it
is normally handled in bulk quantities in plant operations as a liquid.
2.4.1.4 Odor
Pure sulfur is odorless.
Formula Name
alkali metal nitrides
Al aluminum
Al + Cu aluminum + copper
Al + Nb2O5 aluminum + niobium pentoxide
NH3 ammonia
NH4NO3 ammonium nitrate
NH4ClO4 ammonium perchlorate
Ba(BrO3)2·H2O barium bromate
BaC2 barium carbide
Ba(ClO3)2·H2O barium chlorate
Ba(IO3)2 barium iodate
B boron
BrF5 bromine pentafluoride
BrF3 bromine trifluoride
Cd cadmium
Ca calcium
Ca(BrO3)2·H2O calcium bromate
CaC2 calcium carbide
Ca(ClO3)2 calcium chlorate
Ca(ClO)2 calcium hypochlorite
Ca(IO3)2 calcium iodate
Ca3P2 calcium phosphide
Ca + VO + H2O calcium + vanadium oxide + water carbides
Cs3N cesium nitride
C + impurities charcoal
ClO2 chlorine dioxide
ClO chlorine monoxide
ClF3 chlorine trifluoride
ClO3 chlorine trioxide
Cr(ClO)2 chromium oxychloride (chromyl chloride)
CrO3 chromium trioxide (chromic acid) anhydride,
chromic
Cu + x-ClO3 copper + chlorates
As2S3 diarsenic trisulfide
Formula Name
Cl2O dichlorine monoxide
(C2H5)2O diethyl ether
fiberglass + iron filings
F2 fluorine
halogenates
halogenites
halogens
Ag7NO11 heptasilver nitrate octaoxide
CxHy hydrocarbons
In indium
interhalogens
IF5 iodine pentafluoride
IO5 iodine pentoxide
C lampblack (carbon black)
Pb(ClO3)2 lead chlorate
PbCl2 lead chloride
Pb(ClO2)2 lead chlorite
PbCrO4 lead chromate
PbO2 lead dioxide (lead peroxide)
Li lithium
Li + NH3 lithium dissolved in ammonia
Li2C2 lithium carbide
Mg magnesium
Mg(BrO3)2·6H2O magnesium bromate
Mg(ClO3)2 magnesium chlorate
Mg(IO3)2·4H2O magnesium iodate
Hg(NO3)2·H2O mercuric nitrate
HgO mercury(II) oxide (mercuric oxide)
Hg2O mercury(I) oxide (mercurous oxide)
x-C2H metal acetylides of carbides
x-(ClO3)n metal chlorates
x-(zO3)n metal halogenates
x-On metal oxides
metals
RbC2H monorubidium acetylide (rubidium acetylene
carbide)
Ni nickel
Formula Name
NO2 nitrogen dioxide
Os osmium
oxidants
Pd palladium
x-(ClO4)n inorganic perchlorates
x-(MnO4)n permanganates
P phosphorus (phosphorus, red)
P4 phosphorus, white (phosphorus, yellow)
P2O3 phosphorus trioxide
K potassium
KBrO3 potassium bromate (bromic acid)
KClO3 potassium chlorate
KClO potassium chlorite (potassium hypochlorite)
KIO3 potassium iodate
KNO3 + As2S3 potassium nitrate (saltpeter) + arsenic sulfide
K3N potassium nitride
KClO4 potassium perchlorate
KMnO4 potassium permanganate
K + SnI4 potassium + tin(IV) iodide (stannic iodide)
Rh rhodium
Rb rubidium
Se selenium
SeC2 selenium carbide
AgBrO3 silver bromate
AgClO3 silver chlorate
AgClO2 silver chlorite
AgNO3 silver nitrate
Ag2O silver oxide
Na sodium
NaBrO3 sodium bromate
NaClO3 sodium chlorate
NaClO2 sodium chlorite
NaH sodium hydride
NaIO3 sodium iodate
NaNO3 + charcoal sodium nitrate + charcoal
Na2O2 sodium peroxide
Formula Name
Na + SnI4 sodium + tin(IV) iodide (stannic iodide)
SrC2 strontium carbide
SrC2+ Se strontium carbide + selenium
SCl2 sulfur dichloride
(C6H5)4Pb tetraphenyl lead
Tl2O3 thallic oxide (thallium peroxide)
Th thorium
ThC2 thorium carbide
Sn tin
U uranium
UC2 uranium carbide (uranium dicarbide)
Zn zinc
Zn(BrO3)2·6H2O zinc bromate
Zn(ClO3)2 zinc chlorate
Zn(IO3)2 zinc iodate
The primary hazard in handling solid sulfur results from the fact
that sulfur dust suspended in the air ignites easily. Even though
b. Liquid Sulfur
The fire hazards of liquid sulfur result primarily from the low
ignition point of sulfur and from the presence of hydrogen
sulfide.
b. Molten Sulfur
2.4.2 Precautions
1. Employees operating equipment containing molten sulfur should
wear clothing capable of protecting the chest and arms, trousers
without cuffs, high top shoes, safety glasses with side shields, and
heat resistant gloves. When making connections or other changes in
molten sulfur piping, full-face shields (in addition to safety glasses)
and leather protective clothing may be needed.
2.5.1.4 Odor
Ammonia has a pungent odor that can be detected at low
concentrations, 20 to 50 PPM.
Formula Name
C2H4O acetaldehyde
C3H4O acrolein
H8N2O8S2 ammonium peroxo disulfate
Sb antimony
SbH3 antimony hydride
B boron
boron halides
BI3 boron triiodide
BrF5 bromine pentafluoride
HClO3 chloric acid
ClN3 chlorine azide
ClO chlorine monoxide
ClF3 chlorine trifluoride
x-ClO2 chlorites
SiHxCl4-x chlorosilane
CrO3 chromium trioxide (chromic anhydride, chromic
acid)
CrCl2 chromyl chloride
Cl2O dichlorine oxide
C2H4Cl2 + NH3 (liq) ethylene dichloride + liquid ammonia
C2H4O ethylene oxide
Au gold
AuCl3 gold (III) chloride
halogens
C3N6Cl6 hexachloromelamine
H4N2 + Li, Na, etc. hydrazine + alkali metals
HBr hydrogen bromide (hydrobromic acid)
Formula Name
HOCl hypochlorous acid
H2O2 hydrogen peroxide
Mg(ClO4)2 magnesium perchlorate
Hg mercury
HNO3 nitric acid
NO2 nitrogen dioxide (nitrogen peroxide)
N2O4 nitrogen tetraoxide
NCl3 nitrogen trichloride
NF3 nitrogen trifluoride
NO2Cl nitryl chloride
OF2 oxygen difluoride
O2 + Pt oxygen + platinum
P2O5 phosphorus pentoxide
P2O3 phosphorus trioxide
C6H3N3O7 picric acid
K + AsH3 potassium + arsine
KClO3 potassium chlorate
K3Fe(CN)6 potassium ferricyanide
K2Hg(CN)4 potassium mercuric cyanide
K + PH3 potassium + phosphine
K + NaNO2 potassium + sodium nitrite
Ag silver
AgCl silver chloride
AgNO3 silver nitrate
Ag2O silver oxide
Na + CO sodium + carbon monoxide
S sulfur
SCl2 sulfur dichloride
TeCl4 tellurium chloride
tellurium hydropentachloride
(CH3)4N2COH2 tetramethyl ammonium amide
SOCl2 thionyl chloride
N3S4Cl thiotrithiazyl chloride
C3H3N6Cl3 trichloromelamine
O3F2 trioxygen difluoride
b. Moist ammonia will rapidly attack copper, tin, zinc, and their
alloys.
The life hazard from ammonia is due to its damage to the lungs when
inhaled. This material is so irritating that it provides its own warning
well below toxic concentrations. Ammonia can usually be detected
at levels of 20-50 PPM. There will be noticeable irritation of the eyes
and nasal passages when exposed to 100 PPM, severe irritation of
the throat, nasal passages, and upper respiratory tract at 400 PPM,
and severe eye irritation at 700 PPM. At 1700 PPM, there will be
severe coughing and bronchial spasms, and an exposure of
30 minutes or less may be fatal. Concentrations of 5000 PPM and
above are fatal almost immediately, causing serious edema of the
lungs, strangulation, and asphyxiation. (Edema is a condition in
which irritated tissues swell, collect fluid, and slowly excrete a watery
fluid, in this case into the lungs.)
For severe irritation of the eyes, hold the lids open and pour clean water
over the eyeball and lids (or use an eye irrigation fountain). Wash
thoroughly in this fashion for 15 minutes. A physician, preferably an eye
specialist, should be summoned immediately.
2.5.3 Precautions
In this part of the complex, ammonia will usually be found mixed with
hydrogen sulfide. Ammonia will always be present in the following
locations:
1. In the process gas and liquid streams in the Sour Water Stripping
Unit.
3. In the SWS Gas Knock-Out Drum liquids, the TGCU quench water,
and the TGCU Stripper reflux.
4. In the overhead gas from the TGCU Stripper, and possibly in the
TGCU recycle gas.
2.6.1.4 Odor
MDEA has a slight odor of amine.
If MDEA vapors are inhaled, remove the patient to fresh air. A physician
should be consulted.
In case of eye contact, flush the eyes with large amounts of water for at
least 15 minutes. Take the patient to a physician, preferably an eye
specialist, at once.
In case of skin contact, flush the affected area with plenty of water. If
exposure has produced a burn, it should be treated like a thermal burn,
2.6.3 Precautions
1. When handling MDEA, employees should wear protective clothing
resistant to MDEA. The choice of gloves, boots, apron, or full-body
suit will depend on the tasks to be performed. Chemical-resistant
goggles should always be worn.
2.7.1.4 Odor
Sodium hydroxide has no odor, in pure form or when dissolved in
water.
Water Solutions
25 wt% 50 wt%
a. Melting Point: -2°F (-19°C) 50°F (10°C)
b. Boiling Point: 232°F (111°C) 288°F (142°C)
c. Auto-Ignition Temp.: Not combustible Not combustible
d. Flash Point: N/A N/A
e. Specific Gravity: 1.27 1.53
f. Color: Colorless or Colorless or
water-white water-white
Formula Name
C2H2O acetaldehyde
C2H2O2 acetic acid
C2H6O3 acetic anhydride
C3H4O acrolein
C3H3N acrylonitrile
C3H6O allyl alcohol
C3H5Cl allyl chloride
Al aluminum
ClF3 chlorine trifluoride
CHCl3 + CH3OH chloroform + methanol
Formula Name
C3H7ClO2 chlorohydrin (chlorhydrin)
C7H7ClO 4-chloro-2-methylphenol
C7H6ClNO2 chloronitrotoluene
ClHSO3 chlorosulfonic acid (chlorosulfuric acid)
C9H8O cinnamaldehyde
Cu copper
CN4 cyanogen azide
B2H6 diborane (boron hydride)
C2H2Cl2 1,2-dichloroethylene
C2H4F2 difluoroethane
C3H5NO ethylene cyanohydrin (hydracrylonitrile)
C2H2O2 glyoxal
HCl hydrochloric acid (hydrogen chloride)
HF hydrofluoric acid (hydrogen fluoride)
C6H6O2 hydroquinone
Mg magnesium
C4H2O3 maleic anhydride
CH3OH + C6H2Cl4 methanol + tetrachlorobenzene
C7H7NO3 4-methyl-2-nitrophenol
3-methyl-2-penten-4-yn-1-ol
HNO3 nitric acid
C2H5NO2 nitroethane (forms shock-sensitive salts)
CH3NO2 nitromethane (forms shock-sensitive salts)
CxH2x+1NO2 nitroparaffins (forms shock-sensitive salts)
C3H7NO2 nitropropane (forms shock-sensitive salts)
H2SO4 SO3 oleum (fuming sulfuric acid)
C5H12O pentol
P phosphorus
P2O5 phosphorus pentoxide
C3H4O2 ß-propiolactone (2-oxetanone)
strong mineral or organic acids
H2SO4 sulfuric acid
C6H2Cl4 1,2,4,5-tetrachlorobenzene
C4H8O tetrahydrofuran
Sn tin
C2H3Cl3O 1,1,1-trichloroethanol
Formula Name
C2HCl3 trichloroethylene
CCl3NO2 trichloronitromethane
H2O water
Zn zinc
Zr zirconium
Contact with the skin, eyes, nose, or respiratory passages can result
in severe burns and scarring. In the case of eye contact, blindness
can occur rapidly.
In case of eye contact, immediately begin flushing the eyes with large
amounts of water, preferably with an eye wash fountain. Continue
flushing for at least 15 minutes, forcibly holding the eyelids apart and
rotating the eyeball, to ensure complete irrigation of all eye and lid tissue.
A physician, preferably an eye specialist, should be summoned
immediately.
In case of skin contact, immediately flush the affected areas with large
amounts of water. If large areas of the body are contaminated, or if
clothing has been penetrated to the skin, immediately use a safety
shower, preferably removing clothing while under the shower. Continue
flushing the areas for at least 15 minutes. If available, follow the water
flush with a generous application of vinegar or 1% acetic acid solution to
neutralize the residual NaOH. After the acid treatment, apply a good
protective dressing as with any other burn and take the patient to a
physician. Contaminated clothing should be washed before reuse.
Contaminated leather articles (shoes, belts, etc.) should be discarded.
2.7.3 Precautions
1. Employees should wear impervious rubber, neoprene, or vinyl
gloves, boots, and overalls or full-body suits, plus tightly fitting
goggles and face shields.
3. When diluting sodium hydroxide, use agitation (mixing) and add the
concentrated sodium hydroxide to water at a controlled rate to
control the heat of dilution and avoid spattering. Never add water to
sodium hydroxide.
1. Most process gas streams (reactor gases, tailgas, and stack gas).
checked regularly for adequate air flow. The motive steam supply to
the eductors, as well as the steam supply to and condensate from
the ventilation system jacketing, should also be monitored.
Sulfur fires may occur in the tanks. Molten sulfur has an auto-ignition
temperature of approximately 450°F (232°C). This is a spontaneous
reaction; no spark or flame is required. Steam system temperatures
are normally well below the auto-ignition point of sulfur. However,
some iron-sulfur corrosion compounds are unstable and can ignite,
or decompose, at lower temperatures to create localized hot spots
and sulfur burning.
Vessel entry refers to any tank, vessel, equipment, or other enclosed place
where there is a hazard of: 1) a toxic, corrosive, or flammable substance;
Almost all of the vessels in this facility fit at least one of the three categories
mentioned above, due to the potential presence of hydrocarbon gas, caustic or
corrosive chemicals, or toxic H2S and SO2. All vessels should be assumed
unsafe for normal entry until prescribed vessel entry procedures have been
followed.
Consider the precautions advised for vessel entry when gauging tanks,
sampling, and blowing down lines or instruments.
Some or all of the following items should be considered for most vessel entry
jobs:
C. Check all internal lines and liquid traps to verify they are free of hazardous
liquid.
(1) Oxygen - The atmosphere must contain 19.5-23.5% oxygen and the
vessel should have adequate ventilation, either forced or natural.
(3) Toxic fumes - The presence of any toxic fumes requires the use of
respiratory protective equipment, normally an air supplied mask with
F. A safety harness and a lifeline shall be worn by the person entering the
vessel if respiratory equipment is required.
G. Personal protective clothing suitable for the job inside the vessel should
be worn.
The following items should be considered in all work involving lines and valves:
2.11.1 General
1. Know the contents of each line being worked on.
2. Know the pressure ratings of the pipes and fittings. Never install low
pressure connections on high pressure lines.
8. When removing blinds, loosen bolts and allow any pressure to bleed
down. Gas sometimes leaks into the space between the blind and
the valve.
2. Lock out, tag out, and try the pump. All gauges and sight glasses
should be checked for zero readings.
4. The worker should slowly open the bolts on the far side, so that if
there is a spray it will be away from him.
2.12.2 Grounding
1. All electrical equipment is to be grounded.
2.12.4 Fuses
1. Fuses should be replaced only by authorized personnel.
2. Fuse tongs and/or rubber electrical gloves should be used and the
disconnect should be opened. Rubber gloves must always be used
for voltages in excess of 150 volts.
2.12.5 Switching
1. When starting electric motors, handle all switches according to
instructions. Make contact so as to prevent arcs. Stand in a safe
position.
3. Always be certain that hands are dry and that the footing is dry when
operating switches or plugging in electrical appliances.
2. All extension cords should be the grounded type. Before each period
of use, examine extension cords carefully for any failure of the outer
insulation, particularly at terminal points where the cord enters a plug
or a fixture.
2.12.7 Miscellaneous
1. Contact with electrical conductors should be avoided whether they
are energized or not.
2.13.2 Boilers
2.13.2.1 Repair and Maintenance
a. Only boiler inspectors or the State boiler agency should
determine a new setting for safety relief valves. Seals on safety
relief valves should never be removed. If a valve leaks, remove
it to a Code-authorized shop for repairs.
(2) Blank the steam line between the stop valve and the
boiler.
e. After repairs, examine the boiler carefully for tools and other
matter before replacing the manhole cover.
2.13.2.2 Operations
a. Open steam valves very slowly to allow cold lines to heat up
and water to drain out before pressure builds.
2.14.2 Equipment
1. Inspect all gas hoses for leaks each day that they are used.
3. Glassware
2. Always pour acids and caustics into water, never the reverse.
3. If acids or caustics enter the eye, flush with plenty of water and
report for first aid treatment.
A. Hydrogen Sulfide
B. Sulfur Dioxide
C. Sulfur
D. Ammonia
E. Methyldiethanolamine
F. Sodium Hydroxide
HYDROGEN SULFIDE
Trade Names / Synonyms: Hepatic Gas; Hydrosulfuric Acid; Stink Damp; Sulfureted Hydrogen; Sulfur
Hydride
SECTION II - COMPONENTS
Other Contaminants: Methyl Mercaptan; Carbon Disulfide; Oxides of Carbon and Sulfur
Description: Colorless gas at atmospheric temperature and pressure, with the odor of
rotten eggs.
Solubility in Water: 4.2 g/l @ 60°F (15°C), 3.2 g/l @ 78°F (25°C)
Other Solvents Carbon Disulfide, Weak Acids, Ethanol, Gasoline, Kerosene, Crude Oil, Liquid
Sulfur
Other Physical Data: Solubility decreases with increasing temperature or with mechanical
disturbance (agitation), causing evolution of dissolved gas.
HYDROGEN SULFIDE
Fire and Explosion Hazard: Highly flammable gas when exposed to heat, flame, or oxidizers.
Moderate explosion hazard. Gas-air mixtures are explosive. Vapors
are heavier than air, and may travel a considerable distance to a
source of ignition and flash back.
Fire-Fighting Procedures: Extinguish only if flow can be stopped; use water in flooding amounts
as fog. Apply from as far a distance as possible. Avoid breathing
poisonous vapors, keep upwind. Evacuate to a radius of 2500 feet for
uncontrollable fires. Evacuate downwind areas as required for leaks.
Fire-Fighting Phases: Stop flow of gas. Use water to keep fire-exposed containers cool and
to protect personnel effecting the shut off. (NFPA 49, Hazardous
Chemicals Data, 1975).
Acute Exposure - Low concentrations may produce nasal and respiratory tract irritation.
At 50 PPM, anosmia, anoxia, headache, nausea, dizziness, vomiting, confusion,
weakness, ataxia, irritability, and insomnia may occur. Rhinitis, pharyngitis, coughing,
bronchitis, and pneumonitis are also possible. At 500-1000 PPM, coma, convulsions,
and death may occur within 30 minutes. At extremely high concentrations, respiratory
paralysis and death from asphyxia may be immediate. Non-fatal exposures may result
in sequelae including residual cough, cardiac dilation, slow pulse, peripheral neuritis,
albuminuria, amnesia, psychic disturbances, and permanent brain damage.
HYDROGEN SULFIDE
Inhalation: Chronic Exposure - Prolonged or repeated exposure to low concentrations may cause
(continued) hypotension, nausea, anorexia, weight loss, incoordination, and chronic cough.
Prolonged exposure to 250 PPM has led to pulmonary edema.
Acute exposure - 50 PPM for one hour has caused conjunctivitis, pain, lacrimation,
photophobia, and appearance of haloes around lights. Within a few hours or days,
symptoms may progress to keratoconjunctivitis and vesiculation of the corneal
epithelium. Higher concentrations may cause severe irritation, lacrimation, and intense
pain.
Acute Exposure - High vapor concentrations may cause severe irritation of the skin.
Swallowing: Treat symptomatically and supportively. Get medical attention immediately. If vomiting
occurs, keep head lower than hips to prevent aspiration.
Inhalation: Remove from exposure area to fresh air immediately. If breathing has stopped, give
artificial respiration. Maintain airway and blood pressure and administer oxygen if
available. Keep affected person warm and at rest. Administration of oxygen should be
performed by qualified personnel. Get medical attention immediately.
Eye Contact: Wash eyes immediately with large amounts of water, occasionally lifting upper and
lower lids, until no evidence of chemical remains (at least 15-20 minutes). In case of
burns, apply sterile bandages loosely without medication. Get medical attention
immediately.
Skin Contact: Flush affected areas with large amounts of water. Consult a physician for further
treatment.
Antidote: Amyl nitrite or sodium nitrite can be used to aid in the formation of sulfmethemoglobin,
thus removing sulfide from combination in tissues. Pyridoxine 25 mg/kg intravenously,
or 10% urea, 1 g/kg intravenously, has been suggested as a sulfide acceptor.
Administration of antidotes should be performed by qualified medical personnel. The
nitrite antidote is toxic; therapy is dangerous. (Dreisbach, Handbook of Poisoning, 11th
ed.)
HYDROGEN SULFIDE
Decomposition: Thermal decomposition products may include toxic and hazardous hydrogen, sulfur,
and oxides of sulfur.
Polymerization: Hazardous polymerization has not been reported to occur under normal temperatures
and pressures.
HYDROGEN SULFIDE
Shut off ignition sources. Stop leak if you can do it without risk. Use water spray to reduce vapors.
Isolate area until gas has dispersed. No smoking, flames, or flares in hazard area! Keep unnecessary
people away; isolate hazard area and deny entry. Ventilate closed spaces before entering. Evacuate
area endangered by gas.
Water used to knock-down vapors is corrosive and toxic, and should be diked for containment. Add
suitable agent to neutralize to 7 pH prior to disposal.
Ventilation: Provide local exhaust or process enclosure ventilation to meet the published exposure
limits. Ventilation equipment must be explosion-proof.
Respirator: The following respirators and maximum use concentrations are recommendations by the
U.S. Department of Health and Human Services; NIOSH Pocket Guide to Chemical
Hazards or NIOSH Criteria Documents; or, Department of Labor, 29CFR1910,
Subpart Z.
The specific respirator selected must be based on contamination levels found in the work
place and be jointly approved by the National Institute of Occupational Safety and Health
and the Mine Safety and Health Administration.
Hydrogen Sulfide:
100 PPM - Supplied-air respirator.
Self contained breathing apparatus.
Escape - Air-purifying full facepiece respirator (gas mask) with chin-style or front-
or back-mounted canister.
Escape-type self-contained breathing apparatus.
HYDROGEN SULFIDE
Respirator For firefighting and other immediately dangerous to life or health conditions:
(continued):
Self-contained breathing apparatus with full facepiece operated in pressure-demand
or other positive pressure mode.
Clothing: Wear protective clothing. Prevent any possibility of repeated or prolonged vapor contact
with skin.
Eye Protection: Employee must wear splash-proof or dust-resistant safety goggles and a faceshield to
prevent contact with this substance.
Where there is any possibility that an employee's eyes may be exposed to this substance,
the employer shall provide an eye-wash fountain within the immediate work area for
emergency use.
2. Since hydrogen sulfide is heavier than air, it settles when released into the atmosphere and becomes
more concentrated near the ground and in low places.
3. Hydrogen sulfide dissolves in liquid sulfur and is a hazard in storage tanks and pits.
Disclaimer
The information contained herein is believed to be accurate, but is not warranted to be, whether originating within the company or not. Health and safety precautions in this data sheet
may not be adequate for all individuals and/or situations. Recipients are advised to confirm in advance of need that the information is current, applicable, and suitable to their
circumstances. It is the end user’s responsibility to evaluate and use this product safely, and to comply with all applicable laws and regulations. No statement made in this data sheet
shall be construed as a permission or recommendation for use of any product in a manner that might infringe existing patents. No warranty is made, either expressed or implied.
SULFUR DIOXIDE
Trade Names / Synonyms: Sulfurous Acid Anhydride; Sulfurous Anhydride; Sulfurous Oxide;
Sulfur Oxide
SECTION II - COMPONENTS
Solubility in Water: 129 g/l @ 60°F (15°C), 102 g/l @ 68°F (20°C)
SULFUR DIOXIDE
Extinguishing Media: Material is nonflammable. Use what is appropriate to the surrounding fire.
SO2 will form a corrosive acidic mist with water fog or steam.
Fire-Fighting Procedures: Fire fighters must use full protective clothing, eye protection, and self-
contained breathing equipment when this material is involved in a fire
situation.
Inhalation: Chiefly affects the upper respiratory tract and the bronchi, causing irritation, difficulty
with breathing, pulmonary edema, and, at high levels, respiratory paralysis. Short
exposures above 50-100 PPM can be dangerous, and, above 400-500 PPM,
immediately life threatening.
Systemic effects of acute or chronic exposure are not fully known. Statistical evidence
has been reported to show increased pulmonary function impairment at chronic SO2
levels of 1-4 PPM. Mixture with smoke particulate or aerosols may increase the
hazards of SO2 inhalation.
Eye Contact: At 20 PPM and above, irritation and inflammation of the conjunctiva.
Skin Contact: At 10,000 PPM, irritating to moist areas within a few minutes.
SULFUR DIOXIDE
Swallowing: Treat symptomatically and supportively. Get medical attention immediately. If vomiting
occurs, keep head lower than hips to prevent aspiration.
Inhalation: The victim must be carried at once to an uncontaminated atmosphere and effective
artificial respiration started immediately if breathing has ceased. Oxygen (100%)
should be administered (by trained personnel only) as soon as possible after a severe
exposure, preferably against a positive exhalation pressure of 1.25 inches of water.
Eye Contact: If sulfur dioxide has contacted the eyes, they should be washed promptly with large
quantities of water for at least 15 minutes. Chemical neutralizers are not advisable. It
is advisable to irrigate the eyes gently with water at room temperature in order to
minimize additional pain and discomfort. Refer the victim at once to a physician,
preferably an eye specialist.
Skin Contact: On skin contact with sulfur dioxide, use an emergency safety shower at once. Clothing
and shoes contaminated with sulfur dioxide should be removed under the shower.
Sulfur dioxide should be washed off with very large quantities of water. Wash skin
areas with large quantities of soap and water. Do not apply salves or ointments to
chemical burns for 24 hours.
SULFUR DIOXIDE
Polymerization: Hazardous polymerization has not been reported to occur under normal temperatures
and pressures.
Notify safety personnel of significant leaks. Exclude all from area except those assigned to leak and
spill control who are using full protective gear (see Section VIII). Provide ventilation. Locate and control
leakage.
If water is used to knock-down vapors, it will be corrosive and toxic, and should be diked for
containment. Add suitable agent to neutralize to 7 pH prior to disposal.
SULFUR DIOXIDE
Ventilation: Provide local exhaust or process enclosure ventilation to meet the published exposure
limits. (Treatment of exhausted air to remove SO2 may be necessary before discharge
to the outside environment.)
Respirator: For fire fighting and other immediately dangerous to life or health conditions:
Clothing: Wear protective clothing. Prevent any possibility of repeated or prolonged vapor
contact with skin.
Eye Protection: Employee must wear splash-proof or dust-resistant safety goggles and a faceshield to
prevent contact with this substance.
Where there is any possibility that an employee's eyes may be exposed to this
substance, the employer shall provide an eye-wash fountain within the immediate work
area for emergency use.
Disclaimer
The information contained herein is believed to be accurate, but is not warranted to be, whether originating within the company or not. Health and safety precautions in this data sheet
may not be adequate for all individuals and/or situations. Recipients are advised to confirm in advance of need that the information is current, applicable, and suitable to their
circumstances. It is the end user’s responsibility to evaluate and use this product safely, and to comply with all applicable laws and regulations. No statement made in this data sheet
shall be construed as a permission or recommendation for use of any product in a manner that might infringe existing patents. No warranty is made, either expressed or implied.
SULFUR
Trade Names / Synonyms: Asulfa-Supra; Bensulfoid; Brimstone; Colloidal Sulfur; Cosan; Devisulphur;
Flowers of Sulfur; Ground Vocle Sulphur; Hexasul; Kumulus; Microwetsulf;
Precipitated Sulfur; Precipitated Sulphur; S-590; S-594; S-595;
Solid Sulfur; Solid Sulphur; Sublimed Sulfur; Sublimed Sulphur; Sulfex;
Sulfran; Sulphur; Uni350
SECTION II - COMPONENTS
Exposure Limits: The Nuisance Dust TLV should govern exposure to solid sulfur in the absence of
other standards:
Liquid sulfur may release hydrogen sulfide and/or sulfur dioxide as gases. Refer
to the specific Material Safety Data Sheets for these substances giving the
applicable exposure limits.
Description: Solid sulfur is odorless, tasteless, yellow rhombic or monoclinic crystals, lumps,
granules, or powder. Sulfur contaminated with hydrocarbon or carbon may be
orange, green, tan, brown, or black in color. Liquid sulfur is viscous and odorless,
with a color ranging from bright yellow to dark orange (almost red) depending on
temperature. Contaminants (particularly hydrogen sulfide) sometimes give sulfur
the odor of rotten eggs.
SULFUR
Other Physical Data: At temperatures up to about 317°F (158°C), the viscosity of pure liquid sulfur
decreases as the temperature increases. As the temperature increases from
317°F to 370°F (158°C to 188°C), the viscosity of pure liquid sulfur rises rapidly to
a tremendously high maximum, causing the liquid to become a dark, sticky,
plastic material impossible to pump.
Fire and Explosion Hazard: Solid - The primary hazard in handling solid sulfur results from the fact that
sulfur dust suspended in the air ignites easily. Even though the explosion
hazard is considered moderate, an explosion occurring in a confined area
could cause considerable damage.
Liquid - The fire hazards of liquid sulfur result primarily from the low ignition
point of sulfur and from the presence of hydrogen sulfide.
Explosive Limits in Air: Lower: 35 g/m3 (2.9% by wt) Upper: 1400 g/m3 (53% by wt)
Extinguishing Media: Small Fires: Water, dry chemical, soda ash, or sand.
(1987 Emergency Response Guidebook, DOT P 5800.4)
Steam smothering can be used in storage pits and other relatively small
enclosures. Carbon dioxide is also a satisfactory fire extinguishing agent.
Fire-Fighting Procedures: Straight streams of water from a nozzle can scatter molten sulfur and
disperse sulfur dust into the air. Sulfur dust is a moderate explosion hazard
when dispersed in air. As sulfur burns, it generates sulfur dioxide, a toxic
gas. Wear self-contained breathing apparatus.
Unusual Hazards: Small dust explosions may disperse larger quantities of dust into the air,
resulting in a serious explosion, particularly in confined areas.
SULFUR
Swallowing: Acute Exposure - A man has survived ingestion of 60 grams of sulfur over a period of
24 hours. Large doses (15 grams) by mouth may lead to hydrogen sulfide production
in vivo, chiefly due to bacterial action within the colon. Small particles are generally
more toxic than large ones. If high levels of impurities are present, sore throat, nausea,
headache, dullness, and possible unconsciousness may occur.
Inhalation: Irritant.
Acute Exposure - Inhalation of large amounts of dust may cause catarrhal inflammation
of the nasal mucosa which may lead to hyperplasia with abundant nasal secretions.
Tracheobronchitis is a frequent occurrence, with dyspnea, persistent cough, and
expectoration, which may sometimes be streaked with blood.
Acute Exposure - 8 PPM has caused irritation of human eyes. Dust may cause
irritation, redness and pain with lacrimation, photophobia, conjunctivitis, and
blepharoconjunctivitis; cases of damage to the crystalline lens have been reported
with the formation of opacities and even cataract and focal chorioretinitis.
Chronic Exposure - Low levels may cause conjunctivitis. Higher levels may cause
symptoms similar to acute exposure.
SULFUR
Acute Exposure - In highly purified form, the dust is low in irritation effects, but
frequently impurities of hydrogen sulfide are present and may produce irritation or
possibly burns.
Chronic Exposure - Soaps, ointments, gels, and drugs containing sulfur are used as
fungicides and parasiticides in the treatment of cutaneous disorders such as psoriasis,
seborrhea, eczema-dermatitis, and scalp disorders. Sulfur possesses a keratolytic
property which may be the basis of its therapeutic reaction. Prolonged local use of
sulfur may result in characteristic dermatitis venenata, possibly with erythematous and
eczematous lesions and signs of ulceration.
Swallowing: Give water or fluids. Emesis is not necessary. Treat supportively and symptomatically.
If irritation or digestive upset occurs, get medical attention.
Inhalation: Remove from exposure area to fresh air immediately. If breathing has stopped,
perform artificial respiration. Keep person warm and at rest. Get medical attention
immediately.
Eye Contact: Wash eyes immediately with large amounts of water, occasionally lifting upper and
lower lids, until no evidence of chemical remains (approximately 15-20 minutes). Get
medical attention immediately.
Skin Contact: Remove contaminated clothing and shoes immediately. Wash affected area with soap
or mild detergent and large amounts of water until no evidence of chemical remains
(approximately 15-20 minutes). Get medical attention immediately.
SULFUR
SULFUR
SULFUR
SULFUR
Decomposition: Combustion may release toxic oxides of sulfur, some of which may react with air and
moisture to produce corrosive sulfurous and sulfuric acids. Toxic and corrosive
hydrogen sulfide may be generated by molten sulfur.
Polymerization: Hazardous polymerization has not been reported to occur under normal temperatures
and pressures.
SULFUR
Small Spill: Shut off ignition sources. Do not touch spilled material. With clean shovel, place material
into clean, dry container and cover; move containers from spill area.
Large Spill: Shut off ignition sources. Do not touch spilled material. Wet down with water and dike
for later disposal. No smoking, flames, or flares in hazard area! Keep unnecessary
people away. Isolate hazard area and deny entry.
Waste should be mixed with four times its weight of crushed limestone, marble, or shell, and then buried
at a permitted disposal site.
Ventilation: Provide local exhaust or process enclosure ventilation to meet the published exposure
limits. Ventilation equipment must be explosion-proof.
For areas containing sulfur dust, the specific respirator selected must be based on the
contamination levels found in the work place, must not exceed the working limits of
the respirator, and be jointly approved by the National Institute for Occupational Safety
and Health and the Mine Safety and Health Administration.
The following respirators are recommended based on the data found in the Physical
Data and Health Hazard Data sections. They are ranked in order from minimum to
maximum respiratory protection:
SULFUR
Respirator: For firefighting and other immediately dangerous to life or health conditions:
(continued)
Self-contained breathing apparatus with a full facepiece operated in
pressure-demand or other positive pressure mode.
Clothing: Employees operating equipment containing molten sulfur should wear clothing capable
of protecting the chest and arms, trousers without cuffs, and high-top shoes. When
making connections or other changes in molten sulfur piping, leather protective clothing
may be needed.
Gloves: Employee must wear heat-resistant gloves when working with molten sulfur.
Eye Protection: Employee must wear splash-proof or dust-resistant safety goggles to prevent eye
contact with this substance. When making connections or other changes in molten
sulfur piping, full face shields (in addition to safety glasses or goggles) should be worn.
Disclaimer
The information contained herein is believed to be accurate, but is not warranted to be, whether originating within the company or not. Health and safety precautions in this data sheet
may not be adequate for all individuals and/or situations. Recipients are advised to confirm in advance of need that the information is current, applicable, and suitable to their
circumstances. It is the end user’s responsibility to evaluate and use this product safely, and to comply with all applicable laws and regulations. No statement made in this data sheet
shall be construed as a permission or recommendation for use of any product in a manner that might infringe existing patents. No warranty is made, either expressed or implied.
AMMONIA
SECTION I - PRODUCT IDENTIFICATION
SECTION II - COMPONENTS
Other Contaminants:
Description Colorless gas at atmospheric temperature and pressure, with a pungent odor.
Solubility in Water: 579 g/l @ 60°F (15°C), 444 g/l @ 68°F (20°C)
Other Solvents:
AMMONIA
SECTION IV - FIRE AND EXPLOSION INFORMATION
Fire and Explosion Hazard: Ammonia is a low fire hazard when exposed to heat or flame
because it is difficult to ignite. It is a moderate explosion hazard
when exposed to flame or fire. Air-ammonia mixtures can detonate
in a fire.
Fire-Fighting Procedures: Stop flow of gas. Wear self-contained breathing apparatus with a
full facepiece operated in pressure-demand mode and full body
protection when fighting fires.
Inhalation: The life hazard from ammonia is due to its damage to the lungs when inhaled. When
inhaled, ammonia is both an irritant and an asphyxiant, and can cause respiratory
distress. Ammonia can usually be detected at levels of 20-50 PPM. There will be
noticeable irritation of the eyes and nasal passages when exposed to 100 PPM, and
severe irritation of the throat, nasal passages, and upper respiratory tract at 400 PPM.
At 1700 PPM, there will be severe coughing and bronchial spasms, and an exposure of
30 minutes or less may be fatal. Concentrations of 5000 PPM and above are fatal
almost immediately, causing serious edema of the lungs, strangulation, and
asphyxiation.
Eye Contact: This gas is dangerous to the eyes, as it causes irritation at 40-100 PPM. Prolonged
exposure to 700 PPM or more can cause extensive injuries to the eyes - irritation,
hemorrhages, swollen lids, corneal ulcers, even partial or total loss of sight.
Skin Contact: Ammonia will irritate the skin, particularly if the skin is moist, to the point of causing
chemical burns from prolonged exposure.
AMMONIA
SECTION V - HEALTH HAZARD DATA (continued)
Swallowing: Treat symptomatically and supportively. Get medical attention immediately. If vomiting
occurs, keep head lower than hips to prevent aspiration.
Inhalation: Where breathing is weak, administer oxygen or mixtures of carbon dioxide and oxygen,
containing not more than 5% carbon dioxide. It should be administered intermittently
for periods of two minutes over a total time not to exceed fifteen minutes. If breathing
has ceased, start artificial respiration immediately, by trained personnel only. Artificial
respiration, when administered by an inexperienced person, is definitely hazardous
following exposure to ammonia, and should be avoided where possible. The use of a
pulmotor is definitely not recommended as its more violent action will irritate and may
severely injure the lungs. A resuscitator used with oxygen and operated by a trained
person is recommended. Keep the patient warm and still, and get medical attention
immediately.
Eye Contact: Hold the lids open and pour clean water over the eyeball and lids (or use an eye
irrigation fountain). Wash thoroughly in this way for 15 minutes. A doctor, preferably
an eye specialist, should be summoned immediately
Skin Contact: Speed is essential. Strip the ammonia-saturated clothing from the body immediately.
Flood affected areas continuously with clean water for at least 15 minutes. Do not
cover burns with clothing or dressings. Allow them to remain open to the air.
AMMONIA
SECTION VI- REACTIVITY DATA
AMMONIA
SECTION VIII - PROTECTIVE EQUIPMENT TO BE USED
Ventilation: Provide local exhaust or process enclosure ventilation to meet the published exposure
limits. Ventilation equipment must be explosion-proof.
Respirator: If work place exposure limit(s) of product or any component is exceeded (see Section
II), a NIOSH/MSHA approved air supplied respirator is advised in absence of proper
environmental control. OSHA regulations also permit other NIOSH/MSHA respirators
(negative pressure type) under specified conditions (see your safety equipment
supplier). Engineering or administrative controls should be implemented to reduce
exposure.
Clothing: To prevent repeated or prolonged skin contact, wear impervious clothing and boots.
Gloves: Wear resistant gloves such as neoprene, nitrile rubber, butyl rubber.
Eye Protection: Employee must wear splash-proof or dust resistant safety goggles and a faceshield to
prevent contact with this substance.
Where there is any possibility that an employee's eyes may be exposed to this
substance, the employer shall provide an eye-wash fountain within the immediate work
area for emergency use.
DISCLAIMER
The information contained herein is believed to be accurate, but is not warranted to be, whether originating within the company or not. Health and safety precautions in this data
sheet may not be adequate for all individuals and/or situations. Recipients are advised to confirm in advance of need that the information is current, applicable, and suitable to their
circumstances. It is the end user's responsibility to evaluate and use this product safely, and to comply with all applicable laws and regulations. No statement made in this data
sheet shall be construed as a permission or recommendation for use of any product in a manner that might infringe existing patents. No warranty is made, either expressed or
implied.
METHYLDIETHANOLAMINE
SECTION II - COMPONENTS
Other Contaminants: Often stored and transported as an aqueous solution containing about 10% water
by weight.
Other Solvents:
METHYLDIETHANOLAMINE
Swallowing: Single dose oral toxicity is low. The oral LD50 for rats is 4780 mg/kg for MDEA.
Amounts ingested incidental to industrial handling are not likely to cause injury;
however, ingestion of larger amounts may cause injury. Ingestion of MDEA can
cause nausea, vomiting, and abdominal discomfort.
Eye Contact: May cause moderately severe irritation with corneal injury.
Skin Contact: Prolonged or repeated exposure may cause skin irritation, even a burn. A single
prolonged exposure is not likely to result in the material being absorbed through
skin in harmful amounts. The dermal LD50 has not been determined.
Swallowing: Induce vomiting if large amounts are ingested. Consult medical personnel.
Eye Contact: Flush eyes with large amounts of water for at least 15 minutes. Take the patient to a
physician, preferably an eye specialist, at once.
Skin Contact: Flush the affected area with plenty of water. If exposure has produced a burn, it
should be treated like a thermal burn, with treatment based on the physician's
judgement. Contaminated clothing should be removed and washed before reuse.
Contaminated leather articles (shoes, belts, etc.) should be removed and destroyed.
ISSUE DATE: 01/25/95 SUPERSEDES: PAGE 2 OF 3
MATERIAL SAFETY DATA SHEET
METHYLDIETHANOLAMINE
Incompatibilities: Incompatible with strong oxidizers and strong acids. Do not allow
MDEA to contact sodium nitrite (NaNO2) or other nitrosating
agents, as nitrosamines (suspected cancer-causing agents) could
be formed.
Hazardous Decomposition Products: Nitrous oxides, carbon monoxide, and/or carbon dioxide.
Wear suitable protective equipment, especially eye protection. Collect for disposal. Toxic to fish; avoid
discharge to natural waters.
Burn in approved incinerator. Follow all local, state, and federal requirements for disposal.
Respirator: None required in normal use. If irritation of the nose and/or respiratory system is
experienced, use an approved air-purifying respirator.
Clothing: Use protective clothing impervious to this material. Selection of specific items such as
boots, apron, or full-body suit will depend on operation.
Avoid contact with eyes, skin, and clothing when handling and storing MDEA. Wash thoroughly after
handling.
Disclaimer
The information contained herein is believed to be accurate, but is not warranted to be, whether originating within the company or not. Health and safety precautions in this data sheet
may not be adequate for all individuals and/or situations. Recipients are advised to confirm in advance of need that the information is current, applicable, and suitable to their
circumstances. It is the end user’s responsibility to evaluate and use this product safely, and to comply with all applicable laws and regulations. No statement made in this data sheet
shall be construed as a permission or recommendation for use of any product in a manner that might infringe existing patents. No warranty is made, either expressed or implied.
SODIUM HYDROXIDE
Trade Names / Synonyms: Caustic; Caustic Soda; Caustic Soda Liquid; Liquid Caustic; Lye;
Lye Solution; Soda Lye; Sodium Hydrate; Quaker Caustic Blend;
White Caustic
SECTION II - COMPONENTS
Component: Sodium Hydroxide Percent: > 99.0
Other Contaminants: Often stored and transported as an aqueous solution. Common strengths are
25, 50, and 73 weight percent NaOH.
Solubility in Water: At 60°F (15°C), more than 50 wt% will dissolve in water.
Other Solvents:
SODIUM HYDROXIDE
Fire and Explosion Hazard: Sodium hydroxide and its water solutions are not flammable. However,
adding water to NaOH or solutions of NaOH can cause localized
overheating due to its heat of dilution.
Extinguishing Media: Not combustible. Use extinguishing agents as may be suitable for
material in surrounding fire.
Fire-Fighting Procedures: Not combustible. Use clothing and safety equipment as may be suitable
for sodium hydroxide and materials in the surrounding fire.
Swallowing: Acutely toxic if swallowed, causing severe burns and scarring to the mouth,
throat, esophagus, and stomach, and may lead to death. Squamous cell
carcinoma of the esophagus can occur years after the exposure.
Inhalation: Inhalation of dust or mist can cause injury to the entire respiratory tract. The
effects of inhalation depend on the severity of the exposure, ranging from mild
irritation of the mucous membranes to severe pneumonitis.
Eye Contact: Contact with the eyes may cause irritation and, with greater exposure, severe
burns and possible blindness.
Skin Contact: Skin contact may cause burns, frequently with deep ulceration and scarring.
Prolonged contact, even with dilute solutions, can cause tissue damage.
SODIUM HYDROXIDE
Swallowing: Do not induce vomiting - this will cause further damage to the throat and
esophagus. Dilute by giving water to the patient immediately. Vinegar, 1% acetic
acid solution, citrus fruit juices, or 5% citric acid solution may also be administered
to help neutralize the alkaline solution. Follow this with milk, egg white in water, or
milk of magnesia. Keep the patient warm and still, and summon a physician
immediately.
Inhalation: Remove the patient to fresh air at once. If breathing has stopped, begin artificial
respiration immediately. Keep the patient warm and still, and summon a physician
immediately.
Eye Contact: Immediately begin flushing the eyes with large amounts of water, preferably with
an eye wash fountain. Continue flushing for at least 15 minutes, forcibly holding
the eyelids apart and rotating the eyeball, to ensure complete irrigation of all eye
and lid tissue. A physician, preferably an eye specialist, should be summoned
immediately.
Skin Contact: Immediately flush the affected areas with large amounts of water. If large areas of
the body are contaminated, or if clothing has been penetrated to the skin,
immediately use a safety shower, preferably removing clothing while under the
shower. Continue flushing the areas for at least 15 minutes. If available, follow
the water flush with a generous application of vinegar or 1% acetic acid solution to
neutralize the residual NaOH. After the acid treatment, apply a good protective
dressing as with any other burn and take the patient to a physician. Contaminated
clothing should be washed before reuse. Contaminated leather articles (shoes,
belts, etc.) should be discarded.
SODIUM HYDROXIDE
Reactivity: Stable.
Other Hazards: Adding water to sodium hydroxide or sodium hydroxide solutions may cause
localized overheating and spattering.
SODIUM HYDROXIDE
Cleanup personnel must wear proper protective equipment (refer to Section VIII). Completely contain
spilled material with dikes, sandbags, etc., and prevent run-off into ground or surface waters or
sewers. Recover as much material as possible into containers for disposal. Remaining material may
be diluted with water and neutralized with dilute hydrochloric acid. Neutralization products, both liquid
and solid, must be recovered for disposal.
Recovered solids or liquids may be sent to a licensed reclaimer or disposed of in a permitted waste
management facility. Consult federal, state, or local disposal authorities for approved procedures.
Ventilation: Ventilation is not usually required for caustic solutions. Avoid creation of mist or
spray. If present, wear appropriate safety clothing and provide local exhaust
systems.
Respirator: Provide mist protection where applicable. Use NIOSH or MSHA approved
respirators.
Clothing: Employees should wear impervious rubber, neoprene, or vinyl boots, overalls, and/or
full-body suits.
When diluting sodium hydroxide, use agitation (mixing) and add the concentrated sodium hydroxide to
water at a controlled rate to control the heat of dilution and avoid spattering. Never add water to sodium
hydroxide.
Disclaimer
The information contained herein is believed to be accurate, but is not warranted to be, whether originating within the company or not. Health and safety precautions in this data sheet
may not be adequate for all individuals and/or situations. Recipients are advised to confirm in advance of need that the information is current, applicable, and suitable to their
circumstances. It is the end user’s responsibility to evaluate and use this product safely, and to comply with all applicable laws and regulations. No statement made in this data sheet
shall be construed as a permission or recommendation for use of any product in a manner that might infringe existing patents. No warranty is made, either expressed or implied.
2. HAZARDS IDENTIFICATION
Emergency Overview:
Repeated or prolonged exposure may irritate eyes, skin and respiratory system. The product gets hot as it first adsorbs
water.
Form: Spheres
Color: White
Primary Routes of Exposure: Contact with skin and eyes. Exposure may also occur via inhalation or
ingestion if product dust is generated.
Eye Contact: Dust and/or product may cause eye discomfort and/or irritation seen as tearing and reddening.
Inhalation: Exposure to dust particles generated from this material may cause irritation of the respiratory tract.
Irritation may be accompanied by coughing and chest discomfort.
Chronic Effects: Prolonged or repeated inhalation of dust generated from this material may cause lung injury.
3. COMPOSITION/INFORMATION ON INGREDIENTS
INGREDIENT % WEIGHT ACGIH TLV-TWA OSHA PEL-TWA UNITS
& CAS NO.
Aluminum oxide (non-fibrous) <95 1(R) 15 (TD) mg/m3
1344-28-1 5(R)
Water <10 N.E. N.E. N.A.
7732-18-5
Abbreviations:
N.A. - Not Applicable RD - Respirable Dust Fu - Fume IS - Insoluble
N.E. - None Established R - Respirable Fraction I - Inhalable FuD - Fume and Dust
STEL - Short Term Exposure Limit F - Respirable Fibers TD - Total Dust SC - Soluble Compounds
Skin contact: Wash off with soap and plenty of water. If skin irritation persists, call a physician.
After inhalation: Remove the victim into fresh air. If symptoms persist, call a physician.
After ingestion: Drink at least 2 glasses of water. Obtain medical attention. Never give anything by mouth to an
unconscious person.
Notes to physician: This product is a desiccant and generates heat as it adsorbs water. Symptomatic treatment is
advised. The used product can retain material of a hazardous nature. Identify that material and treat symptomatically.
Fire and explosion hazards: The product itself does not burn. The used product can retain material of a hazardous
nature. Identify that material and inform the fire fighters.
Special protective equipment: In the case of respirable dust and/or fumes, use self-contained breathing apparatus and
dust impervious protective suit.
Clean-up: Sweep, shovel or vacuum spilled product into appropriate containers (do not use a vacuum if material has
contacted a hydrocarbon material). Pick-up and arrange disposal without creating dust. Never use spilled product. Spilled
product should be disposed of in accordance with all applicable government regulations.
Personal protection equipment: Handle in accordance with good industrial hygiene and safety practice.
Skin and body protection: Work uniform and gloves to prevent prolonged contact.
Respiratory protection: In case of insufficient ventilation, wear suitable respiratory equipment. Air-purifying
respirator with NIOSH classification N-95 filter or P-95 (or equivalent) if oil/liquid aerosols are present (42 CFR 84).
10. STABILITY
Stability: Stable
Hazardous Decomposition Products: No decomposition if used as directed. Hydrocarbons and other materials that
contact the product during normal use can be retained on the product. It is reasonable to expect that decomposition
products will come from these retained materials of use. If the product is subject to extreme temperatures or chemical
conditions, decomposition may occur and he product will include the oxides shown in Section 3.
Conditions/Materials to avoid: Reacts violently with chlorine trifluoride, producing flames. May cause ethylene oxide
to polymerize violently, releasing heat.
Routes of exposure: Exposure may occur via inhalation, contact with skin and eyes.
Irritation:
Further Information:
No information available.
Disposal information: This product (in its fresh unused state) is not listed by generic name or trademark name in the
U.S. EPA’s RCRA regulations and does not possess ay of the four identifying characteristics of hazardous waste
(ignitability, corrosivity, reactivity or toxicity). Materials of a hazardous nature that contact the product during normal use
may be retained on this product. The user of the product must identify the hazards associated with the retained material
in order to assess the waste disposal options.
Toxic Substances Control Act (TSCA): All the ingredients of this mixture are registered on the TSCA Chemical
Substance Inventory.
CERCLA (Comprehensive Environmental Response, Compensation, and Liability Act) Reportable Quantity:
The following component(s) of this product is/are subject to release reporting under 40 CFR 302 when release exceeds
the Reportable Quantity (RQ):
--None—
Note: Other U.S. State Regulations may exist, check your local sources if available.
Canadian Environmental Protection Act: All the ingredients of this mixture are notified to CEPA and on the DSL
(Domestic Substances List).
European Inventory of Existing Commercial Chemical Substances: All components of this product are included in
EINECS/ELINCS.
Australia – Inventory of Chemical Substances (AICS): All the ingredients of this mixture appear on the AICS.
China – All the ingredients of this mixture appear on the China Inventory.
Japan – Existing and New Chemical Substances (ENCS): All the ingredients of this mixture appear on the
ENCS.
Korea – Existing and Evaluated Chemical Substances (ECL): All the ingredients of this mixture appear on the
ECL.
Philippines – Inventory of Chemicals and Chemical Substances (PICCS): All the ingredients of this mixture
appear on the PICCS.
HEALTH: 1
FLAMMABILITY: 0
REACTIVITY: 1
EMERGENCY OVERVIEW
Physical Appearance: Blue Extrudates or Spheres. Odorless
Human Health Hazards:
Irritating to eyes and respiratory system.
May cause allergic reaction (rash) with skin contact and asthma-like allergic reaction by inhalation in
sensitive individuals.
Physical Hazards:
No specific hazards.
Environmental Hazards:
Toxic to aquatic organisms, may cause long-term adverse effects in the aquatic environment.
Page 1 of 8
CRITERION 234 CATALYST MSDS Number: 6179
Skin:
Mildly irritating to the skin. May cause contact dermatitis (allergic skin rash) in cobalt sensitive
individuals.
Inhalation:
Dusts may be irritating to the nose, throat and respiratory tract. May cause sensitization by inhalation
due to presence of a cobalt compound. Existing respiratory diseases may be aggravated by exposure to
this material.
Ingestion:
Low-level cobalt ingestion is known to cause effects on the heart after a short-term exposure. The
symptoms of heart damage may be a swelling of the feet (edema) and shortness of breath on exertion
or when lying flat on the back (supine).
Skin Contact:
Wash skin with water and, if available, soap. If persistent irritation occurs, get medical attention.
Inhalation:
Move to fresh air. If rapid recovery does not occur, get medical attention.
Ingestion:
Do not induce vomiting. Give nothing by mouth. Get medical attention immediately.
Note to Physicians:
Treat symptomatically. If skin sensitization has developed and a causal relationship has been
confirmed, further exposure should not be allowed.
Spill Management:
Prevent contamination of soil and water. Do not wash spills into sewers or other public water systems.
Prevent further leakage or spillage and prevent from entering drains.
Page 2 of 8
CRITERION 234 CATALYST MSDS Number: 6179
Spill Disposal:
Shovel up and place in a labeled, sealable container for subsequent safe disposal.
Environmental Compliance:
Refer to latest state or local regulations to determine if there are disposal or reporting requirements.
Storage Recommendations:
Keep container tightly closed and dry.
Reseal plastic liner.
Hygiene Measures:
Avoid contact with material. Wash hands thoroughly after handling. Do not reuse clothing if
contaminated until thoroughly decontaminated.
Respiratory Protection:
Use either an atmosphere-supplying respirator or an air-purifying respirator for particulates.
Eye Protection:
Wear safety goggles or glasses to prevent eye contact.
Hand Protection:
Wear neoprene, nitrile, PVC or latex gloves to prevent contact.
Body Protection:
When there is a possibility of exposure wear a one piece coated overall with integral hood, safety
boots, chemical-resistant without lace holes.
Page 3 of 8
CRITERION 234 CATALYST MSDS Number: 6179
Product
Physical & Chemical Properties Characteristics
Appearance and Odor: Blue Extrudates or Spheres. Odorless
Solubility in water: <5%
Bulk density (solids): 0.48 g/cc
Melting point: ~3700
Materials To Avoid:
Strong acids, strong bases, strong oxidizing agents.
Acute Lethality
Route Material Tested LD/LC50 Species
Dermal Molybdenum oxide >2000 mg/kg Rat
Sensitization
Route Material Tested Description Species
Dermal Cobalt oxide Sensitizer Human
Inhalation Cobalt oxide Sensitizer Human
Cobalt was used as a defoaming agent in beer at 1 ppm. After a few weeks of exposure beer drinkers were found
to have myocardial effects. Deaths were reported. Medical evaluations found myocardial infarction.
In a lifetime feeding study with cobalt in hamsters, no statistically significant increases in tumors were seen.
Carcinogenicity:
Cobalt oxide is classified by:
IARC as a possible human carcinogen (Group 2B)
Page 4 of 8
CRITERION 234 CATALYST MSDS Number: 6179
Mobility:
Sinks in water. If product enters soil, one or more constituents will be mobile and may contaminate
groundwater.
Sewage Treatment:
Not toxic at the limit of water solubility.
Waste Disposal:
If product is unused, see above. If used, evaluate the toxicity and physical properties of the material
you have generated and dispose of the material in accordance with local, state and federal regulations.
Container Disposal:
Empty containers may contain residues. Ensure container is properly cleaned. Remove all packaging
for recovery or waste disposal. DO NOT USE CONTAINER FOR OTHER PURPOSES.
Regulatory Controls:
Comply with all federal, state and local laws regulating the handling and disposal of wastes.
Page 5 of 8
CRITERION 234 CATALYST MSDS Number: 6179
National Inventories
National Authority Country Status
EINECS/ELINCS EC All ingredients listed.
TSCA USA All ingredients listed.
MITI Japan All ingredients listed.
DSL/NDSL Canada All ingredients listed.
TCCL Korea All ingredients listed.
AICS Australia All ingredients listed.
PICCS Philippines All ingredients listed.
IECS China All ingredients listed.
California Proposition 65
Name on List Classification
Cobalt oxide Carcinogen
Massachusetts
Aluminum oxide Right-To-Know Substances List
Pennsylvania
Aluminum oxide Right-To-Know Hazardous Substance
Molybdenum oxide PA Environmental Hazard E (1 % threshold)
Page 6 of 8
CRITERION 234 CATALYST MSDS Number: 6179
European Community
Label Name CONTAINS COBALT OXIDE / MOLYBDENUM OXIDE
Hazard Symbols Xn: Harmful
N: Dangerous to the Environment
Classification Harmful Dangerous to the Environment
Risk Phrases R48/20/22: Harmful: danger of serious damage to health by prolonged
exposure through inhalation and if swallowed.
R42/43: May cause sensitization by inhalation and skin contact.
R36/37: Irritating to eyes and respiratory system.
R51/53: Toxic to aquatic organisms, may cause long-term adverse
effects in the aquatic environment.
Safety Phrases S22: Do not breathe dust.
S24: Avoid contact with skin.
S37/39: Wear suitable gloves and eye/face protection.
S61: Avoid release to the environment. Refer to special
instructions/Safety data sheets.
MSDS Distribution:
The information in this document should be made available to all who may handle the product.
Page 7 of 8
CRITERION 234 CATALYST MSDS Number: 6179
Amendment Notation:
Amendments from the previous version of the MSDS are indicated by two vertical bars in the left
margin and the section is highlighted.
Disclaimer:
This information is based on our current knowledge and is intended to describe the product for the
purposes of health, safety and environmental requirements only. It should not, therefore, be construed
as guaranteeing any specific property of the product.
Issue Date:
01/25/2010
US/Canada - (English)
Page 8 of 8
Operating Guidelines Samsung Total Petrochemicals Co., Ltd.
Fall 2011 Daesan, Korea
SULFUR BLOCK
Table of Contents
3. GENERAL .................................................................................................................... 3-1
3.1 ORGANIZATION ................................................................................................... 3-1
3.2 GENERAL PRECOMMISSIONING PROCEDURES ............................................. 3-2
3.2.1 Mechanical ..................................................................................................... 3-2
3.2.2 Electrical ......................................................................................................... 3-3
3.2.3 Instrumentation ............................................................................................... 3-5
3.3 DESIGN BASIS ..................................................................................................... 3-7
3.3.1 Plant Capacity ................................................................................................ 3-7
3.3.2 Sulfur Block Feed Streams ............................................................................. 3-7
3.3.3 Effluent Stream Conditions ........................................................................... 3-12
3.3.4 Other Design Requirements ......................................................................... 3-13
3.3.5 Utility Information .......................................................................................... 3-14
3.3.6 Plant Site Conditions .................................................................................... 3-16
3. GENERAL
3.1 Organization
This manual discusses the startup and operation of the new Sulfur Block,
consisting of an Amine Treating Unit, an Amine Regeneration Unit, a Sour
Water Stripping Unit, two Sulfur Recovery Units, a common Tailgas Thermal
Oxidation Unit, Tailgas Cleanup Unit, and Sulfur Degassing Unit, on a systems
basis. The systems are discussed individually, but are also grouped together
into two main categories. The categories and systems, in order of presentation,
are:
A. UTILITY SYSTEMS
1. Power Distribution
3. Utility Systems
B. PROCESS SYSTEMS
3. Sulfur Recovery
5. Tailgas Cleanup
The systems are presented in the sequence required for a normal startup. That
is, electric power is usually the first system commissioned and the Sulfur
Degassing system is usually the last.
3.2.1 Mechanical
A complete check of all plant construction should be made to assure it is
in accordance with the Piping & Instrument Diagrams and equipment
manufacturer's recommendations. Any discrepancies or defects should
be corrected before attempting to put the plant in operation. Each piece of
equipment should be checked against the vendor's recommendations and
guidelines. Some of the steps that should be taken to ensure the plant is
mechanically ready for startup include:
C. Perform all necessary pressure tests. After tests, remove the test
blinds, giving special attention to those below relief valves.
3.2.2 Electrical
The purpose of commissioning electrical components and control systems
prior to the startup of a plant is to ensure correct performance per
specifications under simulated operating conditions.
WARNING
B. Test the motor feeder with the motor out of the circuit. After motors
are connected, make phase-to-ground tests on the motor circuit.
D. Test the feeders to the panel-boards with the branch circuits open.
E. Test the power feeder with switches and circuit breakers in place.
F. Megger the power and control circuits of the switchgear and motor
control centers.
L. For circuit breakers with adjustable trips, check the thermal rating
against the value shown on the drawings and adjust the magnetic
setting to the "LO" position. On magnetic-only (instantaneous trip)
breakers in combination starters, the instantaneous setting should be
adjusted so that the setting is just above the motor in-rush current.
Lower the setting to the point where the contacts open when the
motor is started, then raise the setting in small increments to the
point where the breaker allows the motor to start.
M. Ensure that all individual motor starter and feeder breakers are in the
"OFF" position.
O. Turn the MCC feeder breakers to the "ON" positions, applying power
to all individual circuit breakers, contactors, and motor switches.
3.2.3 Instrumentation
The purpose of commissioning instruments prior to the startup of the
facility is to ensure correct performance per specifications under simulated
operating conditions. Handling of instruments after calibration should be
kept to a minimum.
C. Once the instrument air system is pressurized, the piping and tubing
should be checked for leaks.
E. "Stroke" the control valves to ensure the valves move in the proper
direction.
H. Check the tag numbers on the steam traps to confirm that each trap
has been installed in the proper location.
Unless stated otherwise, the design conditions presented below are assumed to
be available at the battery limits for the new units.
Temp, °C 38
Press, kg/cm2(g) 6
Temp, °C 63 41
Press, kg/cm2(g) 4.5 4.5
Temp, °C 52 55 54 60 38
Press,
kg/cm2(g) 3.0 3.0 3.0 3.0 3.0
Note (1) The maximum NHT sour water rate is 19585 kg/h containing 35 wt
ppm H2S and 18 wt ppm NH3 when running 100% NWS Narrow
feed.
Treated Fuel
Composition, mole %
Gas
Hydrogen 67.353
H2S 0.010
Water Vapor 1.067
Methane 2.729
Ethane 2.180
Propane 1.948
i-Butane 0.988
n-Butane 13.306
i-Pentane 6.633
n-Pentane 3.481
C6 + 0.305
Totals 100.000
Temperature, °C 38
Temperature, °C 40
3.3.4.2 The Rich Amine from the DHT, LPG Absorber and Amine Treating
Unit will go to the Amine Regeneration Unit for regeneration. The
maximum Rich Amine loading will be 0.40 mole acid gas / mole
MDEA.
3.3.4.4 In general, the Sulfur Block is to be designed for a 3-4 year run
length between turnarounds. Mechanical turnaround duration is
usually 3-7 days for each unit.
3.3.5.2 Steam
Operating Pressure: Operating Temp. Mechanical
kg/cm²(g) °C Design
Press: Temp:
Min Norm Max Min Norm Max kg/cm²(g) °C
HP Steam 44 45 46 380 400 420 50 427
MP Steam 16 17 17.5 275 280 300 20 350
IP Steam 13.7 14.4 15.1 202 204 206 16.7 227
LP Steam 3 3.5 4 190 195 210 5.5 300
3.3.5.3 Condensate
HP Steam HP Condensate 19
MP Steam MP Condensate 6
IP Steam LP Condensate 1.5
LP Steam LP Condensate 1.5
Composition, mole %
Nitrogen 99.5
Oxygen 20 ppmv (max)
CO 20 ppmv (max)
CO2 20 ppmv (max)
Other C Compounds 5 ppmv (max)
Chlorine 1 ppmv (max)
H2O 5 ppmv (max)
Hydrogen 20 ppmv (max)
Noble Gases Remainder
Total 100.0
Table of Contents
4. POWER DISTRIBUTION .............................................................................................. 4-1
4.1 PURPOSE OF SYSTEM ....................................................................................... 4-1
4.2 SAFETY ................................................................................................................. 4-1
4.2.1 General ........................................................................................................... 4-1
4.2.2 Hazardous (Classified) Areas ......................................................................... 4-1
4.3 EQUIPMENT DESCRIPTION ................................................................................ 4-2
4.3.1 Motors and Motor Controls ............................................................................. 4-2
4. POWER DISTRIBUTION
4.1 Purpose of System
This utility system supplies electrical power to all users in the Amine Treating,
Amine Regeneration, Sour Water Stripping, Sulfur Recovery, Tailgas Cleanup,
Tailgas Thermal Oxidation, and Sulfur Degassing units including motors,
instruments, controls, lights, receptacles, and heat tracing.
4.2 Safety
4.2.1 General
Only authorized and qualified personnel should maintain and repair
electrical equipment. All operator controls and adjustments are accessible
without opening electrical equipment enclosures.
Table of Contents
5. PLANT CONTROL SYSTEMS ..................................................................................... 5-1
5.1 DISTRIBUTED CONTROL SYSTEM .................................................................... 5-1
5.2 PROGRAMMABLE LOGIC CONTROL SYSTEM ................................................. 5-2
5.3 EMERGENCY SHUTDOWN SYSTEMS ............................................................... 5-3
5.4 LOCAL CONTROL PANELS ................................................................................. 5-3
The safety system interlocks and sequential control functions are performed by a
programmable logic controller (PLC). A PLC is a solid-state microprocessor that
performs the functions of a traditional relay logic system. The PLC for the new units
will communicate with the DCS to allow the operator to monitor the PLC using the
operator interface screens of the DCS.
The system has been designed so that control and monitoring functions are
distributed on a modular basis to minimize control and data information loss in
the event of a failure anywhere within the system. Control functionality does not
depend on a single centrally-based device or communication system to assure
that on a single failure the system will remain operative to allow continued
control and monitoring of the remainder of the process. To achieve this,
redundancy has been included for controllers, power supplies, communication
modules and cables, and operator workstations.
The PLC hardware and programs are fail-safe by design. Loss of power to the
PLC will de-energize all its outputs and send devices (control valves, etc.) to
their "fail" position. The restoration of power to the PLC will restart the PLC, but
program interlocks will "lock-out" control actions until the respective ESD
systems are reset. Similarly, the PLC logic has been designed such that open
circuits in field wiring or open field contacts will de-energize their respective
outputs and render equipment and process to a "safe" status.
The PLC system is connected by both "hard-wired" cables and software "links"
that allow it to communicate with the DCS. This enables the DCS operator
interface to be used by the operators to monitor the status of the PLC and its
safety and sequential control systems.
These ESD systems are mostly independent of each other, with the exception of
the TGCU ESD system, which is activated when both of the SRU ESD systems
are activated. Except for this situation, activation of the ESD system in a
particular unit will not cause any other ESD systems to be directly activated. Of
course, depending on the particular circumstances, the effects that result when
a particular ESD system is activated may indirectly cause another ESD system
to be activated due to the process upset that occurs.
Table of Contents
6. UTILITY SYSTEMS ...................................................................................................... 6-1
6.1 PURPOSE OF SYSTEM ....................................................................................... 6-1
6.2 SYSTEM DESCRIPTION ...................................................................................... 6-1
6.2.1 Nitrogen Supply .............................................................................................. 6-1
6.2.2 C4 LPG and Treated Fuel Gas Supply .......................................................... 6-2
6.2.3 Hydrogen Supply ............................................................................................ 6-2
6.2.4 Plant Air .......................................................................................................... 6-3
6.2.5 Instrument Air ................................................................................................. 6-3
6.2.6 Sour Water Disposal....................................................................................... 6-3
6.2.7 Steam, Condensate, Boiler Feed Water, and Blowdown ............................... 6-4
6.2.7.1 Purpose of Systems ................................................................................ 6-4
6.2.7.2 Safety ...................................................................................................... 6-4
6.2.7.3 Process Description ................................................................................ 6-5
6.2.7.4 Boiler Feed Water ................................................................................... 6-5
6.2.7.5 HP Steam ................................................................................................ 6-6
6.2.7.6 LP Steam................................................................................................. 6-7
6.2.7.7 Condensate Return ................................................................................. 6-7
6.3 PRECOMMISSIONING, STARTUP, AND SHUTDOWN PROCEDURES............. 6-8
6. UTILITY SYSTEMS
6.1 Purpose of System
The utility headers supply the fluids necessary for plant operation and
maintenance.
Nitrogen is also used for several other purposes within the new units: 1) to
purge instruments (flame scanners, pyrometers, flow meters, etc.)
exposed to process gas containing sulfur vapor or ammonia; 2) to empty
out and purge vessels before opening them for maintenance; 3) to prevent
a vacuum from forming in several overhead lines; 4) as the motive fluid for
the aspirator in the air demand analyzer; and 5) as a cool-down medium
for the SRUs and the front-end of the TGCU. A dedicated low pressure
header is used for purges permanently connected to low pressure sulfur
plant equipment; a high pressure header operating at about 7.0 kg/cm2(g)
provides nitrogen for the other users.
The pilot burners for the Acid Gas Burner and the Thermal Oxidizer
Burner are not as reliable if variable quality fuel gas is used. For this
reason, vaporized LPG is used for both pilots to ensure reliable light-off
and good service life.
During normal operation, loss of the treated fuel gas supply will cause the
Thermal Oxidizer to shut down. However, the SRU should continue to
operate. The Thermal Oxidizer shutdown will be due to "flame failure" of
the Thermal Oxidizer Burner. Loss of LPG will normally not affect either
unit, but it will not be possible to restart either unit should a shutdown
occur until the LPG supply is restored.
Sour water must also be drained from equipment items periodically (pump
cases, level instruments, etc.). The Closed Drain Tank, A2-FA1582, has
an underground header system to collect these liquids and hold them. As
the tank fills, the Closed Drain Pump, A2-GA1581A/B, can be used to
send the collected sour water to Sour Water Stripping Unit.
WARNING
THE LIQUID DRAINED INTO THE CLOSED DRAIN TANK AND ITS
UNDERGROUND HEADER SYSTEM CONTAINS DISSOLVED H2S.
ALWAYS OBSERVE PROPER PROCEDURES AND PRECAUTIONS
WHEN DRAINING LIQUID FROM THESE ITEMS OR PERFORMING
MAINTENANCE ON THEM. THE "GENERAL SAFETY" SECTION
OF THIS MANUAL SHOULD BE CONSULTED IF THERE IS ANY
DOUBT ABOUT HOW TO WORK SAFELY WHEN H2S MAY BE
PRESENT.
6.2.7.2 Safety
Use appropriate safety precautions when handling the boiler feed
water chemicals (sulfite, amine, phosphate, etc.).
In accordance with the ASME Section VIII Code for Unfired Steam
Boilers, boiler feed water must be provided to the Sulfur Condenser,
A2-EA1531 (A2-EA1541), and the TGCU Waste Heat Reclaimer,
A2-EA1561, at 5.8 kg/cm2(g)or higher (i.e., 6% above the relief valve
settings).
6.2.7.5 HP Steam
The Waste Heat Boiler, A2-BF1530 (A2-BF1540), generates
HP steam at a normal operating pressure of about 48.5 kg/cm2(g). A
small portion of this steam is consumed in the reactor feed heaters to
reheat the feed streams to the catalytic reactors in the SRUs. The
rest of the HP steam is combined with the steam from the Thermal
Oxidizer Waste Heat Boiler, A2-BF1570, enters the Steam
Knock-Out Drum, A2-FA1570, to remove any entrained water
droplets, and is then routed to the superheat passes in the Thermal
Oxidizer Waste Heat Boiler.
Note that the Thermal Oxidizer Waste Heat Boiler is the only source
of superheat for the HP steam produced in the Sulfur Block. If the
Thermal Oxidizer shuts down and begins to cool, the steam will no
longer be sufficiently superheated to satisfy the requirements of the
users located outside of battery limits. Under this circumstance, the
steam from the superheat passes of the TTO Waste Heat Boiler will
instead be vented to atmosphere automatically until the Thermal
Oxidizer is restarted and the steam is once again superheated to the
proper temperature.
HP steam is used as motive fluid for the Sulfur Surge Tank Vent
Ejector, A2-EE1530 (A2-EE1540). The steam for this service is
normally supplied from the steam produced within the process train.
When the HP steam is being vented to atmosphere as described
above, however, steam must be imported into the Sulfur Block for
this equipment item.
6.2.7.6 LP Steam
The Sulfur Condenser, A2-EA1531 (A2-EA1541), in the sulfur plant
and the TGCU Waste Heat Reclaimer, A2-EA1561, in the tailgas
cleanup unit generate LP steam at a normal operating pressure of
about 4.2 kg/cm2(g). This LP Steam is used for heating amine acid
gas in the Acid Gas Preheater, A2-EA1530 (A2-EA1540), reboiling
the solvent in the ARU Stripper Reboiler, A2-EA1512A/B, the water
in the Sour Water Stripper Reboiler, A2-EA1521, and the TGCU
solvent in the TGCU Stripper Reboiler, A2-EA1565, miscellaneous
steam tracing and steam jacketing of process gas lines, sulfur
rundown lines, sulfur vapor valves, etc., and for the heating coils in
the Sulfur Surge Tank, A2-EA1531 (A2-EA1531), and Sulfur Storage
Tank, A2-FB1550. The remaining LP Steam is exported to the
refinery.
Table of Contents
7. AMINE TREATING & AMINE REGENERATION ......................................................... 7-1
7.1 PURPOSE OF SYSTEM ....................................................................................... 7-1
7.2 SAFETY ................................................................................................................. 7-1
7.3 PROCESS DESCRIPTION.................................................................................... 7-2
7.3.1 General ........................................................................................................... 7-2
7.3.2 Water Washing ............................................................................................... 7-2
7.3.3 Sour Gas Contacting ...................................................................................... 7-3
7.3.4 Solvent Regeneration ..................................................................................... 7-3
7.4 EQUIPMENT DESCRIPTION ................................................................................ 7-6
7.4.1 Wash Water Column, A2-DA1510 .................................................................. 7-6
7.4.2 Amine Absorber, A2-DA1511 ......................................................................... 7-6
7.4.3 Flash Gas Contactor, A2-DA1512 .................................................................. 7-6
7.4.4 Stripper, A2-DA1513 ...................................................................................... 7-6
7.4.5 Wash Water Column Packing, A2-DB1510 .................................................... 7-7
7.4.6 Amine Absorber Trays, A2-DB1511 ............................................................... 7-7
7.4.7 Stripper Trays, A2-DB1513 ............................................................................ 7-7
7.4.8 Amine Absorber Overhead Cooler, A2-EA1510 ............................................. 7-8
7.4.9 Lean/Rich Exchanger, A2-EA1511A/B ........................................................... 7-8
7.4.10 Stripper Reboiler, A2-EA1512A/B .................................................................. 7-8
7.4.11 Stripper Reflux Condenser, A2-EC1511......................................................... 7-8
7.4.12 Lean Amine Cooler, A2-EC1510 .................................................................... 7-8
7.4.13 Wash Water Feed Knock-Out Drum, A2-FA1510 ........................................... 7-8
7.4.14 Amine Absorber Feed Knock-Out Drum, A2-FA1511 ..................................... 7-9
7.4.15 Amine Absorber Overhead Knock-Out Drum, A2-FA1512 ............................. 7-9
7.4.16 Rich Amine Flash Drum, A2-FA1513 ............................................................. 7-9
7.4.17 Stripper Reflux Accumulator, A2-FA1514..................................................... 7-10
7.4.18 Stripper Reboiler Condensate Pot, A2-FA1515A/B ...................................... 7-10
7.4.19 ATU Skim Oil Sump, A2-FA1516 ................................................................. 7-10
7.4.20 ATU Skim Oil Pump Sump, A2-FA1517A/B ................................................. 7-10
7.4.21 ATU Amine Drips Tank, A2-FA1580............................................................. 7-11
7.4.22 MDEA Storage Tank, A2-FB1580 ................................................................ 7-11
7.4.23 Wash Water Filter, A2-FD1510A/B ............................................................... 7-11
7.4.24 Rich Amine Filter, A2-FD1511A/B ................................................................ 7-11
7.4.25 Lean Amine Filter, A2-FD1512 ..................................................................... 7-11
7.4.26 Lean Amine Carbon Filter, A2-FD1513 ........................................................ 7-12
7.4.27 Lean Amine After-Filter, A2-FD1514 ............................................................ 7-12
7.4.28 ATU Amine Drips Filter, A2-FD1580 ............................................................ 7-12
The purpose of the Amine Regeneration system is to strip the H2S from the
rich amine solvent produced in the Amine Treating, LPG Treating and DHT
units. The H2S-laden acid gas is sent to the Sulfur Recovery Unit (SRU) for
disposal and the lean amine is recycled back to the upstream process units.
7.2 Safety
WARNING
The Amine Treating Unit (ATU) uses an aqueous amine solvent, MDEA
(methyldiethanolamine), to remove essentially all the H2S from the sour
fuel gas stream. The normal solvent concentration is 45 wt % MDEA in
water. The ATU is designed to treat 10,397 Nm3/hr of sour fuel gas. The
treated gas stream is returned to the refinery for consumption as fuel, and
the acid gas (H2S, plus CO2) is routed to the Sulfur Recovery Units
(SRUs). Less than 100 PPMV of H2S remains in the treated fuel gas.
The sour fuel gas enters Wash Water Feed Knock-out Drum, A2-FA1510,
at 38°C [100°F] and 6.0 kg/cm2(g) [85 PSIG]. Any entrained liquids are
removed automatically on level control and routed to the sour liquids
system. The scrubbed gas enters the bottom of the Wash Water Column,
A2-DA1510, and passes upward through a packed bed where it is
countercurrently contacted with a stream of circulating water. The washed
sour gas stream leaves the top of the column and flows to Amine
Absorber Feed Knock-out Drum, A2-FA1511, to remove any wash water
that may be carried over with the gas. The scrubbed gas proceeds to the
Amine Absorber, A2-DA1511, while any wash water carry-over is routed
to the Closed Drain system on level control.
The wash water leaving the bottom of the column is pumped by the Wash
Water Pump, A2-GA1510A/B, to the Wash Water Filter, A2-FD1510A/B,
for removal of any particulates or other solid material removed from the
sour gas feed. Most of the filtered water is returned to the top of Wash
Water Column on flow control, after being mixed with fresh makeup water.
The remainder of the filtered water is directed to the Sour Water Stripping
Unit (SWS) to purge the gaseous and liquid contaminants removed by the
wash water from the system. The makeup water rate can be adjusted as
necessary to control the contaminants (primarily ammonia in most cases)
at an acceptable concentration, and the level control on the column
bottoms will automatically adjust the purge rate to balance the water
added to the system with the makeup water flow control.
After removal of any liquid hydrocarbon, the heavier amine phase passes
under the internal weir at the outlet end of the drum to be pumped through
the Rich Amine Filter, A2-FD1511A/B, by the Rich Amine Pump,
A2-GA1513A/B, on level/flow cascade control. The filter removes
particulates from the solvent before it enters the tube side of the
Lean/Rich Amine Exchanger, A2-EA1511A/B. The Rich Amine is
preheated to 105°C [221°F] by cooling the lean solvent before flowing to
the Stripper, A2-DA1513, entering between trays #4 and #5.
along with the uncondensed water) stripped from the solvent exits the
reflux drum at 0.85 kg/cm2(g) [12 PSIG] and flows to the SRUs.
A small stream of cool lean amine is directed on flow control to the top of
the Flash Gas Contactor as described previously. A portion of the cool
lean amine flows to the LPG Treating Unit and a portion flows to the DHT
unit on temperature control. The remaining lean amine is pumped to
higher pressure by the Lean Amine Pump, A2-GA1511A/B before being
directed on flow control to the top of the Amine Absorber.
A chimney tray is located below the bottom valve tray to gather all of the
column liquids to feed the Stripper Reboiler. The column section located
below this chimney tray serves to separate the outlet steam and lean
amine from the reboiler and to provide surge for the solvent circulating
system.
Gaskets are installed where the bed support and distributor tray bolt to the
support ring and clips inside the Wash Water Column to prevent direct
contact between the stainless steel internals and the carbon steel vessel.
This electrically isolates the dissimilar metals from each other to prevent
direct contact that could lead to galvanic corrosion.
The chimney tray gathers the tower liquids to feed the reboiler. The outlet
from the reboiler reenters the column below the chimney tray, with the
vapor produced by the reboiler flowing upward through the chimneys in
order to reach the valve trays above.
The top four trays in the column are located above the rich amine feed
point and serve as water-wash trays to minimize the amount of amine
carried-over in the tower overhead. Since these trays have only the reflux
water flowing over them, the liquid rates for these trays are much lower
than for the trays lower in the column. For this reason, these four trays
are designed for minimum leakage (i.e., picket fence weirs, minimum
downcomer clearance, etc.).
As stated above, this vessel is simply a very good steam trap. During
normal operation, the steam pressure required to provide the necessary
reboil heat to the Stripper may be much less than the 3.5-4.2 kg/cm2(g)
steam pressure available in the LP steam system. The normal steam
pressure in the shell of the reboiler may be such that the water level in the
condensate pot will rise upwards from the pot, perhaps even within the
shell of the reboiler. During these periods, the level valve will remain fully
open and the sight glass will indicate a full water level. This is a normal
operating condition for this vessel. The vessel will usually operate with a
visible level only when the Stripper Reboiler is operating near its
maximum capacity with full steam pressure on the shell of the exchanger.
Under these conditions, the level control and level valve will function
normally and maintain a water level in the vessel.
WARNING
CAUTION
WARNING
THE LIQUID IN THESE PUMPS CONTAINS DISSOLVED H2S. THIS H2S CAN
BE RELEASED TO THE SURROUNDINGS WHEN LIQUID IS DRAINED FROM
THESE PUMPS OR FROM THE PIPING CONNECTED TO THE PUMPS.
ALWAYS OBSERVE PROPER PROCEDURES AND PRECAUTIONS WHEN
DRAINING LIQUID FROM THESE PUMPS OR PERFORMING MAINTENANCE
ON THEM. THE "GENERAL SAFETY" SECTION OF THESE GUIDELINES
SHOULD BE CONSULTED IF THERE IS ANY DOUBT ABOUT HOW TO WORK
SAFELY WHEN H2S MAY BE PRESENT.
If the solvent level drops too low in the Amine Absorber, large
amounts of high pressure gas could blow through control valve
A2-LV15040 into the Rich Solvent Flash Drum, A2-FA1513, and
other equipment and piping in the ATU/ARU with a lower design
pressure than this column. Loss of solvent in this column could
also result in the treated fuel gas going sour.
When S/D valve A2-NV15002 closes to stop the gas flow into the
ATU, the pressure of the incoming sour fuel gas will begin to rise.
When it reaches the setpoint (6.3 kg/cm2(g)) of over-ride pressure
controller A2-PC15001, the controller will open control valve
A2-PV15001 to divert the sour gas to the flare header.
1. Low temperature
5. Intimate contacting
In general practice, items 4 and 5 are not operating variables, having been
fixed by the design criteria for the unit and choice of equipment in the
absorber design.
CAUTION
The withdrawal of lean amine from the bottom of the Stripper is on flow
control to the Amine Absorber. As a result, the level in the bottom of the
Stripper, which serves as the "surge" for the system, will usually indicate if
adjustments of water makeup to the amine system (or water "bleed" from
the system) are required to maintain the proper water balance, as
discussed later in Section 7.6.3 Even if water must be bled from the
system by diverting some of the column reflux to Sour Water Stripping, the
amine content of that waste stream should be low and only infrequent
makeup of fresh amine should be required.
There is full-flow of rich amine through the Rich Amine Filter, and full-flow
of lean amine flow through the Lean Amine Filter, the Lean Amine Carbon
Filter, and the Lean Amine After-Filter. These four filters will remove
solids and organic contaminants from the circulating amine, such as
degradation or corrosion products. The filter elements should be changed
as soon as the "change" pressure drop is reached, to remove as many
solids from the amine as possible. Finely divided solids can cause
foaming and thereby limit column capacity. While it is possible to reduce
foaming to some extent with anti-foam agents, the presence of such
agents may also reduce H2S/CO2 selectivity in the Amine Absorber, so it
is preferable that they not be used as an alternative to regular
conscientious filter maintenance
1. The water content of the feed gas to the Amine Absorber (the
overhead from the Wash Water Column).
3. The water content of the acid gas leaving the Stripper Reflux
Accumulator.
For given operating pressures, the water content of each gas stream will
be determined by the temperature at the top of the respective vessel
(Water Wash Column, Amine Absorber, and Stripper Reflux Accumulator,
respectively), and will increase as the temperature increases. Since the
Amine Absorber inlet gas is at a slightly higher pressure than the outlet
treated gas, the inlet gas will normally contain less water than is contained
in the outlet gas (if both gas streams are at the same temperature), thus
requiring water makeup to maintain the proper water content of the amine.
This situation will be reversed if the Amine Absorber overhead
temperature is lower than the Wash Water Column overhead temperature,
requiring a "bleed" of water to maintain water balance.
Since the lean amine to the Amine Absorber is on flow control and
withdrawal of the rich amine from the bottom of the Amine Absorber is on
level control, a net gain or loss in the amine water balance will be reflected
by an increase or decrease, respectively, of the liquid level in the bottom
of the Stripper. Observation of this liquid level can thus guide adjustment
of water makeup/bleed rate or operating conditions to maintain the desired
water concentration of the circulating amine. Since the degree of H2S
removal can depend on the amine concentration of the amine, the
concentration should be maintained close to the design value (45 wt %)
by appropriate maintenance of water concentration. It is usually possible
to control the water balance without adding fresh water or "bleeding" water
to the Sour Water Stripping Unit by adjusting the operating temperatures
in the unit, as discussed in the following paragraphs. Following the steps
outlined below will allow controlling the water balance with minimum
usage of treated makeup water and minimum impact on the sour water
system.
(1) Begin "bleeding" water (or increase the "bleed" water rate) from
the amine system with the flow controller on the discharge line
of the Stripper Reflux Pump.
CAUTION
This will increase the amount of water leaving in the fuel gas,
and it will also reduce the H2S-removal capability of the solvent.
An increase in solvent flow rate will probably be needed to
maintain the same H2S content in the vent gas, increasing the
load on the Stripper and the other process equipment
associated with the circulating solvent.
Although this will increase the water content of this stream and
reduce the water in the solvent, the effect will be small because
the quantity of acid gas is small relative to the fuel gas. This
adjustment is the least effective and would not normally be
considered during routine operations.
3. Decrease the acid gas temperature with the aerial cooling from
the Stripper Reflux Condenser to reduce the water loss in the
stream as much as possible.
4. Begin water makeup (or increase the makeup water rate) to the
solvent system using the make-up flow controller to add
condensate to the system..
Amine degradation occurs via reactions with acids which can enter the
Amine Absorber when the Wash Water Column is experiencing an upset.
Any traces of acid entering the Amine Absorber will react with the MDEA
to form a thermally non-regenerable complex (i.e., heat-stable salt). If
present in sufficient quantity, this salt can alter the H2S-amine equilibrium
and prevent removal of H2S to the desired level in the Amine Absorber
overhead. Heat-stable salts also increase the corrosivity of the amine.
Amine quality can be restored by treatment with an amount of caustic
equivalent to the non-regenerable salt present but, if repeated caustic
Amine losses due to entrainment in the treated fuel gas or the acid gas
can be minimized by proper process operation (avoidance of column
overloading, foaming, etc.) and routine inspection of the vessel internals.
Amine losses in the water "bleed" from the Stripper reflux should be
negligible if the rectifying trays (the "wash water" trays above the amine
feed point) in the Stripper are operating properly (no flooding or foaming,
no mechanical damage).
The primary source of amine loss will likely be the mechanical losses from
pump drips, cleaning of filters, etc. Good housekeeping practices,
including prompt replacement or repair of leaking pumps, together with
proper collection of amine drips for reuse (via the ATU Drips Tank,
A2-FA1580), will minimize the mechanical loss of amine.
In the case of the Wash Water Column, decrease the wash water rate in
proportion with the gas flow rate down to about 50% of design should
maintain adequate performance. (It should be noted, however, that there
is really no detrimental effect if the wash water circulation is simply left at
the design value at all times. The only drawback is slightly higher power
consumption by the pump and aerial cooler.)
In the packed Amine Absorber, circulating more amine relative to the gas
flow rate should maintain performance. The liquid flow rate should be
maintained at a minimum of about 50%.
C. Check the rotation of the fans on the Lean Amine Cooler and the
Stripper Reflux Condenser, by operating each fan for a short period.
D. Check all piping and equipment to be sure that all blinds have been
removed and that no valves are vented to atmosphere.
F. Check all relief valves to ensure that they are installed in the proper
locations, the inlet and outlet block valves (if provided) are open, the
bypass valves (if provided) are closed, and the relief valves are set
for the correct relieving pressure.
C. Check all relief valves to ensure that they are installed in the proper
locations and set for the correct relieving pressures.
D. The low-low level shutdowns for the pumps in the wash water and
amine systems will be tested while washing these systems as
described in the following sections.
This same procedure can be used to leak test the ATU following
maintenance, before restarting the unit. Whenever plant maintenance
requires opening one or more of the flanged connections in the ATU it is
good practice to leak test the unit before returning it to service. This
allows detecting any leaking connections that may have resulted from the
maintenance operations before sour fuel gas is reintroduced into the unit.
A. Reduce the output from the sour fuel gas hand control in the DCS to
0% to close the Sour Fuel Gas inlet valve.
B. Confirm that the Wash Water Column is isolated from the wash water
circulation loop by confirming that the following valves are all closed:
(1) The bypass valve and downstream block valve at the wash
water flow control valve.
(4) The bypass valve and downstream block valve at the make-up
water flow control valve.
(1) The bypass valve and downstream block valve at the lean
solvent flow control valve.
(2) The bypass valve and upstream block valve at the Absorber
level control valve.
(5) The bypass valve and upstream block valve at the Absorber
overhead pressure control valve to the SRUs.
(6) The bypass valve and upstream block valve at the Absorber
overhead pressure control valve to the flare.
Due to the volume inside the ATU, it will take several minutes for the
pressure to build up in the unit.
F. Once the desired pressure has been achieved close the valve where
the nitrogen "jumper" is connected to stop the flow of nitrogen. Check
all of the equipment and piping connections for visible or audible
signs of leakage.
Failure to clean the system properly prior to startup can lead to operating
problems (heat exchanger fouling, rapid filter plugging, etc.).
WARNING
C. Confirm that the Sour Fuel Gas inlet hand control in the DCS is
set to 0% output so that the Sour Fuel Gas inlet valve is fully
closed.
D. Verify that the Wash Water flow control valve is fully open.
Open both of its isolation block valves and its bypass valve.
E. Verify that the Wash Water Column level control valve is fully
closed. Close both of its isolation block valves and its bypass
valve.
F. Verify that the Sour Fuel Gas inlet valve is fully closed. (This
will prevent water from entering the upstream equipment if the
Wash Water Column is accidentally over-filled.)
G. The Wash Water Filters will not be used to filter solids during
this time, but the filter vessels and their piping are to be flushed
and cleaned. Remove the filter elements, then bolt-up the
filters. Open the inlet and outlet block valves on the filters, and
open the bypass valve around the filters.
H. Add water to the top of the Wash Water Column by placing the
Make-up Water flow control valve in manual and setting its
output to 100% to fully open the make-up water flow control
valve.
J. Watch the level in the Wash Water Column while placing the
pump in service to be sure the pump does not lose suction
while filling the downstream piping and equipment. If the level
disappears in the column, shut the pump down until enough
water (or condensate) is added to reestablish the level, then
restart the pump.
L. Use the low point drain valves to flush out each section of the
system. Leave the drain valves open until the water is clear.
M. Briefly open the bypass valve on the Wash Water Column level
control valve to flush this section of piping to The Sour Water
Stripping Unit. Open the upstream block valve, open the Wash
Water Column level control valve with the level controller in the
DCS, and use the downstream drain valve to flush the control
station. Once the flush water clears up, close the Wash Water
Column level control valve and the upstream block valve.
N. Circulate the water and blow down the low point drains until all
of the drain water is clear. Add more water ( or condensate) as
necessary to maintain the level in the Wash Water Column.
P. Allow the pump to continue running while the system drains, but
watch the pump closely to verify that the low-low level shutdown
shuts the pump down below the shutdown setpoint. If the level
drops completely out of the gauge glass before the pump shuts
down, stop the pump manually and correct the problem with the
low-low level shutdown before proceeding further.
D. After circulating for about 3 hours, start the other Wash Water
Pump and shut down the first one.
F. Briefly open the bypass valve on the Wash Water Column level
control valve to flush this section of piping to The Sour Water
Stripping Unit. Then open both block valves and use the level
controller in the DCS to open the Wash Water Column level
control valve briefly and flush the control station. Close the
Wash Water Column level control valve and the block valves.
G. After 6 hours, shut down the pump and completely drain the
system. Drain the system as quickly as possible, so that the
liquid velocity will help flush any remaining solids from the
system.
E. After circulating for about 1 hour, start the other Wash Water
Pump and shut down the first one.
G. Briefly open the bypass valve on the Wash Water Column level
control valve to flush this section of piping to the sour water
header. Then open both block valves and use the level
H. After 2 hours, shut down the pump and completely drain the
system. Drain the system as quickly as possible, so that the
liquid velocity will help flush any remaining solids from the
system.
A. Close the inlet and outlet block valves on the Wash Water
Filters (but leave the bypass valve open), then install the proper
element(s) in the filters. Leave the block valves closed for now.
(2) "Crack" the filter inlet block valves open slightly and allow
the filters to fill with water. When the filter is full, close the
vent valve.
(3) Open the filter inlet block valves fully and open the outlet
block valves, then close the filter bypass valve.
E. Place the Wash Water flow controller in the DCS in service and
set its setpoint to its normal value. Close the bypass valve on
the Wash Water flow control valve.
The Wash Water system is now ready for service. It can remain in
this operating mode indefinitely while the rest of the ATU is prepared
for startup. Check the system periodically for indications of plugging,
etc. (low flow, erratic pump discharge pressure, high filter pressure
drop), as solid materials may accumulate at various points in the
system over time.
Failure to clean the system properly prior to startup can lead to operating
problems (column foaming, poor treating, heat exchanger fouling, rapid
filter plugging, etc.).
WARNING
(1) Set the output from the lean solvent flow controller to
100% to fully open the lean solvent flow control valve.
(2) Open the manual block valve upstream of the lean solvent
filters.
(3) Set the output from the lean solvent filter bypass flow
controller to 100% to fully open the filter bypass flow
control valve.
(4) Set the output from the Amine Absorber level controller to
100% to fully open the Amine Absorber level control valve.
(5) Set the output from the Rich Amine flow controller to 100%
to fully open the rich amine flow control valve.
(6) Set the output from the amine flow controller to the Flash
Gas Contactor to 100% to fully open the flow control valve.
(7) Set the output from the Stripper Reboiler steam flow
controller to 0% to fully close the steam flow control valve.
(8) Set the output from the Stripper Reflux Accumulator level
controller to 0% to fully close the Stripper Reflux
Accumulator level control valve.
(9) Set the output from the bleed water flow controller to 0% to
fully close the bleed water flow control valve.
(10) Set the output from the flow controller on the spill-back line
to the lean amine cooler to 0% to fully close the spill-back
flow control valve.
(11) Set the output from the makeup water flow controller to 0%
to fully close the makeup water flow control valve.
(14) Set the output from the lean solvent flow controller to the
LPG Treating Unit to 0% to fully close the lean solvent flow
control valve to the LPG Treating Unit.
C. Verify that the following control valves are fully open. Open
both of the isolation block valves and the bypass valve (where
applicable) at each control station.
(3) The Amine Absorber level control, (the rich solvent from
the Amine Absorber).
(4) The rich solvent flow control (the rich solvent from the Rich
Amine Flash tank)
D. Verify that the following control valves are fully closed. Close
both of the isolation block valves and the bypass valve at each
control station.
(3) The bleed water flow control valve from the Stripper reflux.
E. Verify that the bypass valve on the pressure control valve to the
flare is closed. Open both of the isolation block valves at this
control station.
F. The solvent filters will not be used to filter solids during this
time, but the filter vessels and their piping are to be flushed and
cleaned. Remove the filter elements, then bolt-up the individual
filters. Open the inlet and outlet block valves on each filter, and
open the bypass valves for the filters.
G. Verify that the valves in the amine makeup line are closed.
Watch the level in the Amine Absorber and the Rich Amine
Flash Tank as the pump fills the downstream piping and begins
to fill the Stripper. When the level drops to the low-low level
shutdown it should shut down the pump. If it does not, stop the
pump manually before it loses suction and correct the problem
with the low level shutdown before proceeding.
P. At this point, neither the flow into or the level of the Amine
Absorber is being controlled. Both control stations are in
"manual" with the valves fully open to flush the piping as much
as possible. Depending on the hydraulics of the system, it may
be necessary to place either or both of these controls in
"automatic" to prevent losing the level in one of the columns. If
so, leave the bypass valve on the control station "cracked" so
that the bypass piping gets flushed.
Q. Use the low point drain valves to flush out each section of the
system. Leave the drain valves open until the water is clear.
R. Circulate the water and blow down the low point drains until all
of the drain water is clear. Add more condensate as necessary
to maintain the levels in the columns.
S. Once the drain water is clear, shut down the Rich Amine Pump
and completely drain the system. Drain the system as quickly
as possible, so that the water velocity will help flush the solids
from all parts of the system.
T. Allow the Lean Amine Pump and the Lean Amine Booster
Pump to continue running while the system drains, but watch
the pumps closely to verify that the Stripper low-low level
shutdown shuts the pumps down when the level falls to the
shutdown setpoint. If the level drops completely out of the
gauge glass before the pumps shut down, stop the pumps
manually and correct the problem with the low level shutdown
before proceeding further.
U. Confirm that the solvent transfer line (for MDEA makeup) has
been flushed and is ready for service.
D. It is unlikely that any steam will leave the top of the Stripper
during this operation, so the Stripper Reflux Accumulator should
remain dry. If a level should develop in this vessel, drain the
water from the vessel using a drain valve on one of the Stripper
Reflux Pumps.
E. After circulating for about 3 hours, start the other Rich Amine
Pump and shut down the first one. Do the same with the Lean
Amine Pumps and the Lean Amine Booster Pumps.
F. Open the flow control valve in the spill-back line to the Lean
Amine Cooler and circulate through this section of piping. Then
close the control valve.
H. After 6 hours, shut off the steam to the Stripper Reboiler, shut
down the pumps, and completely drain the system. Drain the
system as quickly as possible, so that the liquid velocity will
help flush any remaining solids from the system.
J. Switch to the other pumps for a few minutes, then shut down
the pumps and completely drain the system.
Q. Once the reflux loop has cleared up (the drain water is clear),
shut off the steam to the Stripper Reboiler, shut down the
pumps, and completely drain the system. Drain the system as
quickly as possible, so that the liquid velocity will help flush any
remaining solids from the system.
H. During another pumping cycle, flush out the bleed water piping
by setting the output of the bleed water flow controller to 100%
to fully open the bleed water flow control valve, opening its
upstream and downstream block valves, and opening its
bypass valve. Then close the valves and set the output of the
bleed water flow control valve back to 0%.
J. Once the solution drained from all the low point drain valves is
clear, shut off the steam to the Stripper Reboiler, shut down the
pumps, and completely drain the system. Drain the system as
quickly as possible, so that the liquid velocity will help flush any
remaining solids from the system.
L. Open the control valve in the spill-back line to the Lean Amine
Cooler for a few minutes, then close the control valve.
M. Switch to the other pumps for a few minutes, then shut down
the pumps and completely drain the system.
A. Close the inlet and outlet block valves (but leave the bypass
valves open) on the solvent filters, then install the proper
elements and/or carbon in the filters. Leave the block valves
closed on each filter for now.
F. Open the high point vent valve on the Stripper overhead line
and allow the steam to purge any air from the vessel. As the
pressure builds, the vent valve can be closed.
H. Ensure that the fans are running on the Lean Amine Cooler and
the Stripper Condenser.
L. If the control loops on the solvent have not already been placed
in service, do so at this time. Switch the Amine Absorber level
controller, and the lean solvent flow controller in the DCS to
"automatic" with their setpoints set to their normal values.
N. Place the level controller for the Rich Amine Flash Tank in
service as follows:
(4) The setpoint of the level controller will be set at the last
reading. Adjust the setpoint to its normal value.
(2) "Crack" the filter inlet block valve open slightly and allow
the filter to fill with solvent. When the filter is full, close its
vent valve.
(3) Open the inlet and outlet block valves on the filter.
(4) Slowly close the valve in the bypass line around the filter.
The solvent system is now ready for service. It can remain in this
operating mode indefinitely while the rest of the Sulfur Block is
prepared for startup. Check the system periodically for indications of
plugging, etc. (low flow, erratic pump discharge pressure, high filter
pressure drop), as solid materials may accumulate at various points
in the system over time.
The Wash Water system and perhaps the amine system have been
cleaned and loaded with their respective initial fills of water and amine.
(The amine system may be waiting on purging of the Amine Absorber
before the system is loaded with amine.)
A. Reduce the output from the Sour Fuel Gas hand control in the
DCS to 0% to close the Sour Fuel Gas inlet valve.
B. Confirm that the Wash Water Column is isolated from the wash
water circulation loop by confirming that the following valves are
all closed:
(1) The bypass valve and downstream block valve at the lean
solvent flow control valve.
D. Open all of the vent valves on the PI and PDT taps on the
Wash Water Column and the Amine Absorber, and the vent
valves at the tops of the columns.
NOTE: If the initial solvent fill was not loaded into the solvent
system earlier to avoid exposing the MDEA to oxygen, this
can be accomplished now. Follow the procedure given in
the previous section to fill the solvent system with its initial
solvent charge.
B. The Wash Water system should be charged with its initial fill of
water, so that the level in the Wash Water Column is at the normal
setpoint for the Wash Water Column level controller.
E. The amine system should be charged with its initial fill of amine, with
the level control in the DCS controlling the level in the Amine
Absorber at its normal setpoint and the level control in the DCS
controlling the level in the Rich Amine Flash Tank at its normal
setpoint.
H. The fans should be operating on the Lean Amine Cooler, with the
temperature controllers on the lean amine controlling at their normal
setpoints.
J. The lean amine filters should be in service, with the bypass flow
controller controlling at its normal setpoint.
L. The overhead temperature from the Stripper should be above the low
temperature alarm point for the temperature indicator.
Before introducing sour fuel gas into the columns, confirm that the proper
operating conditions have been established for the Wash Water and
amine systems.
If any of the proper conditions have not been established, do not proceed
until correcting the problem(s). Once all of the conditions are satisfied,
complete the startup of the as follows:
A. Confirm that the sour fuel gas inlet hand control in the DCS is set to
0% output with the Sour Fuel Gas Inlet Valve closed.
B. Slowly increase the output from the sour fuel gas inlet hand control
to 100%, which will open the Sour Fuel Gas Inlet Valve and admit
sour fuel gas to the Wash Water Column.
C. When the output of the sour fuel gas inlet hand control reaches
100%, the Sour Fuel Gas Inlet Valve should be fully open and the
pressure control valve to the flare should be closed to send all of the
sour fuel gas into the Wash Water Column. Visually confirm that
these valves are properly positioned.
D. Once the operation of the Stripper has stabilized, route its acid gas,
which is presently going to the flare through a pressure valve, to the
SRUs as follows:
The Stripper pressure controller will now take over control of the
Stripper pressure by opening the pressure valve to send the acid gas
to the Acid Gas Knock-Out Drum in the SRUs. The Stripper
pressure controller to the flare will close the acid gas pressure valve
and stop the flow of acid gas to the flare. If the SRUs shut down (or
some other upset causes the Stripper pressure to rise), the Stripper
pressure controller to the flare will act as an over-ride and divert the
acid gas to the flare.
(2) The steam heating systems are in service and the level
control on the Reboiler condensate pot is functioning
properly.
If the ARU must also be shut down, then more extensive procedures must be
followed to accomplish a satisfactory shutdown and minimize the time required
for performance of the desired maintenance work. Section 7.9.2 that follows is
an example of a procedure for this circumstance.
The ATU/ARU is affected directly and indirectly by shutdowns and outages that
occur in other systems within the complex. The more important aspects of the
effects these other systems can have on the ATU/ARU are discussed in
Section 7.9.4.
Typical shutdown procedures are outlined and discussed in the sections that
follow for the more common cases. Your existing company procedures and
common sense operational judgment should be used to modify these
procedures as needed to serve the purpose of any given planned shutdown
situation.
A. Slowly reduce the output from the Sour Fuel Gas hand control in the
DCS. As the pressure in the sour fuel gas inlet line begins to
increase, the override pressure controller will open the pressure
control valve and begin diverting the sour fuel gas to the flare
system.
B. When the output of the Sour Fuel Gas hand control reaches 0%, the
pressure control valve should be open and the Sour Fuel Gas inlet
valve should be fully closed to send all of the sour fuel gas to the
flare system.
C. Allow the amine to continue to circulate until the all of the H2S and
CO2 have been stripped from the amine. Once the H2S/CO2 content
of the "rich" amine leaving the Absorber is essentially the same as
the "lean" amine, the ATU can be shut down and isolated from the
ARU.
(3) Place the Wash Water Column level controller in the DCS
in "manual" and set its output to 0% to fully close the level
control valve.
(5) Verify that the wash water flow control valve is fully closed.
Close both of its isolation block valves and its bypass
valve.
(6) Verify that the Wash Water Column level control valve is
fully closed. Close both of its isolation block valves and its
bypass valve.
(7) Verify that the make-up water flow control valve is fully
closed. Close both of its isolation block valves and its
bypass valve.
E. Once the H2S/CO2 content of the "rich" amine leaving the Absorber is
essentially the same as the "lean" amine, the ATU can be shut down
as follows:
(3) Place the amine make-up water flow controller in the DCS
in "manual" and set its output to 0% to fully close the
amine make-up water flow control valve.
(5) Allow the amine to drain from the Amine Absorber until the
low-low level shutdown is activated. This should close the
level control valve. Monitor the level in the Amine Absorber
(6) Monitor the level in the Rich Amine Flash Tank to ensure
that rich amine does not spill over into the hydrocarbon
section of the vessel. Be prepared to take action and close
the Amine Absorber level control valve if the amine level
gets too high in the Rich Amine Flash Tank.
(8) Verify that the Amine Absorber level control valve is fully
closed. Close both of its isolation block valves and its
bypass valve.
(9) Verify that the lean amine flow control valve is fully closed.
Close both of its isolation block valves and its bypass
valve.
(10) Verify that the make-up water flow control valve is fully
closed. Close both of its isolation block valves and its
bypass valve.
(11) Verify that the spill-back flow control valve is fully closed.
Close both of its isolation block valves and its bypass
valve.
F. The ATU is now ready to be isolated and made safe for entry.
A. Shutdown and isolate the DHT Unit and the LPG Treating Unit using
the operating procedures for those units.
B. Slowly reduce the output from the Sour Fuel Gas hand control in the
DCS. As the pressure in the sour fuel gas inlet line begins to
increase, the pressure controller will open the pressure control valve
and begin diverting the sour fuel gas to the flare system.
C. When the output of the Sour Fuel Gas hand control reaches 0%, the
pressure control valve should be open and the Sour Fuel Gas inlet
valve should be fully closed to send all of the sour fuel gas to the
flare system.
E. Continue to circulate the amine and operate the Lean Amine Cooler
and the Stripper Reflux Condenser until the amine is cool.
(3) Place the Wash Water Column level controller in the DCS
in "manual" and set its output to 0% to fully close the level
control valve.
(5) Verify that the wash water flow control valve is fully closed.
Close both of its isolation block valves and its bypass
valve.
(6) Verify that the Wash Water Column level control valve is
fully closed. Close both of its isolation block valves and its
bypass valve.
(7) Verify that the make-up water flow control valve is fully
closed. Close both of its isolation block valves and its
bypass valve.
G. Once the amine is cool (60°C or less throughout the system), shut
down the equipment in the following order:
(5) The fans on the Lean Amine Cooler and Stripper Reflux
Condenser.
H. The ATU and ARU are now ready to be isolated and made safe for
entry.
1
The Dow Chemical Company, Gas Conditioning Fact Book, 1962, pp. 310-311.
2
Dow Chemical U.S.A., Gas Treating from Dow, 1987, pp. 8-1-1 – 8-1-2.
Heat stable salts can also be determined by a total anion assay. The
amine solution is passed through an ion exchange column containing ion
exchange resin in the hydrogen form. Acid salts are thus broken down
and the acids recovered in the column effluent, while the amine is
absorbed in the column. The acid in the effluent is determined by
potentiometric titration, and from these results plus the original amine
concentration the amount of amine in the form of heat stable salts is
calculated. Again, this type of analysis is commonly left for the chemical
solvent supplier to perform.
Steps should be taken to ensure that the amine solution samples taken
are representative of the circulating solvent. Samples should be taken in
glass or plastic containers. Metal containers will cause low results for H2S
because sulfides will react with the metal walls of the container. Do not
use copper tubing to withdraw the samples; the copper will contaminate
the amine solution, and H2S will react with the copper and give low
results.
Special care should be exercised when taking samples of the rich amine
solution to avoid personnel exposure to H2S. Hot, fully loaded amine
solution can flash acid gas when released to atmospheric pressure,
causing low acid gas loading results in addition to the dispersion of H2S to
the surroundings. Take samples of the rich solution from the coolest point
in the process (the Amine Absorber outlet, usually), and cool the samples
in a stainless steel coil immersed in an ice bath or cold water to prevent
flashing. The solution should be allowed to flow to a drain in this fashion
for several minutes before taking the sample to be sure that circulating
amine is being taken.
2. Procedure:
d. Titrate the solution in the beaker with 0.5 N HCl to a faint yellow
color. Alternatively, if a pH meter is available, titrate to a pH of
4.5. Record the amount of HCl used in the titration.
2. Procedure:
hydrogen carbonate salts. Once all of the acid gas has reacted, the
continued addition of base causes the pH of the solution to rise, until
the Thymolphthalein indicator changes from colorless to blue. Note
that KOH reacts with H2S and CO2 on a 1:1 molar basis.
Note that "ml KOH used" refers to the amount used in the second
titration, step 2.e. The "wt % amine in solvent" can be determined
using the procedure in Section 7.10.2.
5. Special Considerations:
2. Procedure:
H2S + I2 S + 2 HI
When the solvent is added to the iodine solution, the H2S in the
solvent reacts with the iodine to form hydrogen iodide and elemental
sulfur. The solution contains an excess of iodine to ensure that all of
the H2S reacts. The iodine solution is chilled prior to adding the
solvent to eliminate or minimize the evolution of H2S gas. Note that
H2S reacts with iodine on a 1:1 molar basis.
g - moles g - moles
Amine I2 Used Na2S2O3 Used
Mole 100 %
Moles H2S
Mole Amine Weight ml of S.G. of Wt % Amine
Sample Sample in Solvent
Normality Normality of
ml I2 of I ml Na2S2O3 Na S O
Used 2 Used 2 2 3
Moles H2S Solution Solution
5.626
Mole Amine ml of Wt % Amine
Sample in Solvent
Using the total acid gas loading determined with the procedure in
Section 7.10.3, the CO2 loading of the solvent is determined by
difference:
Moles H2S
Wt % Amine
Wt % H2S 0.2858
Mole Amine in Sample
Moles CO2
Wt % Amine
Wt % CO2 0.3693
Mole Amine in Sample
1. Principle:
3. Procedure:
c. Start the air pump or air supply to agitate the sample with
oil-free air at 4 liters per minute (0.2 Nm3/H).
d. After five minutes, record the height of the foam in the cylinder
(in ml). Then turn off the air supply and measure the time in
seconds for the foam to "break". For consistency, foam "break"
is defined as the first clear "fish eye" in the surface of the liquid
in the cylinder.
4. Calculation:
5. Interpretation:
Considerable experience with this test has shown that if the foam
height exceeds 200 ml or the "break" time exceeds 5 seconds, the
plant may be experiencing a foaming problem. The higher the foam
height and/or the longer it takes to "break", the more severe the
problem.
6. Other Considerations:
H2S + I2 2 HI + S
The Normality of the standard iodine solution will be 0.1 N. The last
three factors (which correct the actual H2S content to compensate for
expansion due to temperature, pressure, and water content) can be
combined and calculated as a function of temperature only. This has
been done for the 500-ml gas sample and is included as the
Tutweiler Factor Chart in Section 7.10.3 of these guidelines
(Chart 2). Therefore, the equation above can be simplified to:
7.10.7 H2S Conc. in Amine Absorber Ovhd Using Gas Detector Tubes
As an alternative to the traditional wet-chemistry method described in the
preceding Section 7.10.6 for determining the concentration of H2S in the
Amine Absorber overhead gas, gas detector tubes can be used to quickly
and easily make this determination. Although the discussion that follows
specifically addresses using gas detector tubes manufactured by
Drägerwerk AG of West Germany, there may be suitable detector tubes
available from other manufacturers. Dräger tubes can be purchased from
most safety equipment supply companies.
c. Break off the tips at each end of a Dräger tube and insert it into
the sample pump (with the arrow on the side of the tube
pointing toward the pump).
e. Stroke the sample pump one time (be sure to compress the
bellows until reaching the stops) and allow the pump to draw
the gas sample into the detector tube. The sample stroke is
complete when the metal chain on the bellows is taut.
f. Close the sample valve and remove the rubber tubing from the
end of the Dräger tube and from the sample valve.
g. Read the length of the brown stain using the marks on the tube
and record the reading.
7.10.7.3 Calculations
Mole (or Volume) PPM H2S (wet basis):
PPM H2S
Stain
Tube 1013
Length Factor Baro. Pres., mbar
The last factor corrects the measurement for pressure effects when
samples are taken at elevations above sea level. Note that the
average barometric pressure at the compex is
14.7 PSIA = 1013 mbar.
The "Tube Factor" depends on the type of Dräger tube used and the
number of sample strokes:
Table of Contents
8. SOUR WATER STRIPPING ......................................................................................... 8-1
8.1 PURPOSE OF SYSTEM ....................................................................................... 8-1
8.2 SAFETY ................................................................................................................. 8-1
8.3 PROCESS DESCRIPTION.................................................................................... 8-2
8.3.1 General ........................................................................................................... 8-2
8.3.2 Sour Water Collection..................................................................................... 8-2
8.3.3 Sour Water Stripping ...................................................................................... 8-3
8.4 EQUIPMENT DESCRIPTION ................................................................................ 8-5
8.4.1 Sour Water Stripper, A2-DA1520 ................................................................... 8-5
8.4.2 Sour Water Stripper Packing and Internals, A2-DB1520 ................................ 8-5
8.4.3 Stripper Trays, A2-DB1521 ............................................................................ 8-5
8.4.4 SWS Cross Exchanger, A2-EA1520 .............................................................. 8-5
8.4.5 Sour Water Stripper Reboiler, A2-EA1521 ..................................................... 8-6
8.4.6 SWS Quench Water Cooler, A2-EC1520 ....................................................... 8-6
8.4.7 SWS Bottoms Cooler, A2-EC1521 ................................................................. 8-6
8.4.8 Sour Water Flash Drum, A2-FA1520.............................................................. 8-6
8.4.9 SWS Skim Oil Sump, A2-FA1522 .................................................................. 8-7
8.4.10 SWS Skim Oil Pump Sump, A2-FA1523A/B .................................................. 8-7
8.4.11 Sour Water Tank, A2-FB1520 ........................................................................ 8-7
8.4.12 Sour Water Filter, A2-FD1520A/B .................................................................. 8-7
8.4.13 Sour Water Transfer Pump, A2-GA1520A/B .................................................. 8-7
8.4.14 SWS Feed Pump, A2-GA1521A/B ................................................................. 8-8
8.4.15 SWS Quench Water Pump, A2-GA1522A/B .................................................. 8-8
8.4.16 SWS Bottoms Pump, A2-GA1523A/B ............................................................ 8-8
8.4.17 SWS Skim Oil Pump, A2-GA1524A/B ............................................................ 8-8
8.5 INSTRUMENTATION AND CONTROL SYSTEMS ............................................... 8-9
8.5.1 SWS Shutdowns and Alarms ......................................................................... 8-9
8.6 PROCESS PRINCIPLES AND OPERATING TECHNIQUES ............................. 8-11
8.6.1 SWS Stripper Operation ............................................................................... 8-11
8.6.2 Quench Water Circulation ............................................................................ 8-12
8.6.3 pH Control .................................................................................................... 8-13
8.7 PRECOMMISSIONING PROCEDURES ............................................................. 8-14
8.7.1 Preliminary Check-out .................................................................................. 8-14
8.7.2 Washing the Sour Water System ................................................................. 8-15
8.8 STARTUP PROCEDURES.................................................................................. 8-19
8.8.1 Initial Startup of the SWS ............................................................................. 8-19
8.8.1.1 Initial Water Fill ...................................................................................... 8-19
8.2 Safety
WARNING
The Sour Water Stripping Unit (SWS) receives sour water streams
containing ammonia (NH3) and hydrogen sulfide (H2S) from other units in
the No. 2 Aromatics Complex. These sour water streams are combined
with sour water produced in the Sulfur Block (predominately Sour Water
from the ATU and excess quench water from the SWS) and steam
stripped to remove essentially all of the NH3 and H2S from the water. The
resulting treated water (containing less than 20 PPMW of H2S and less
than 20 PPMW of NH3) is returned to the complex for reuse elsewhere,
while the SWS off-gas (NH3, H2S, and water vapor) is routed to the SRUs.
After removal of any liquid hydrocarbon, the heavier water phase passes
under the internal weir at the outlet end of the drum to be pumped to the
Sour Water Tank, A2-FB1520, by the Sour Water Transfer Pump,
A2-GA1520A/B, on level control. This tank is large enough to provide
3-4 days of residence time to allow "working off " an accumulation of sour
water after an outage. The tank also provides time for mixing which
minimizes Sour Water Stripper feed composition fluctuations due to the
many sources of sour water in the complex.
Traditional reflux systems do not work well for strippers in this service
because of the highly corrosion nature of concentrated NH3-H2S aqueous
systems. For this reason, these systems often employ a direct-contact
condenser instead, using a circulating stream of quench water to provide
cooling for the upper section of the column. The Sour Water Stripper
contains an upper section of packing to provide contact between the
quench water and the stripped gases, and a lower section of valve trays to
provide contact between the sour water and the stripping steam.
The stripping section of the column contains 30 valve trays and one
chimney draw tray. As the sour water flows down the column, the NH3
and H2S are stripped from the water by countercurrent contact with
stripping steam rising upward. This stripping steam is generated in the
Sour Water Stripper Reboiler, A2-EA1521, using LP (3.5 kg/cm2(g)
[50 PSIG]) steam on flow control as the heat input. The stripping steam
strips the NH3 and H2S from the water and carries it upward to the quench
section of the column. The SWS Bottoms Pump, A2-GA1523A/B, pumps
the treated water from the bottom of the column through the shell side of
the SWS Cross Exchanger, cooling the treated water from 123°C [254°F]
to 54°C [130°F] by countercurrent heat exchange with the cool sour
water. The SWS Bottoms Cooler, A2-EC1521, provides final cooling to
49°C [120°F] before the treated water is returned to the complex for reuse
elsewhere.
The quench section of the column contains a packed bed and a chimney
draw tray. As the stripping steam rises upward in this section, it is
countercurrently contacted by the circulating quench water, cooling the
off-gas to 85°C [185°F] as it condenses most of the steam. The chimney
tray below the packed bed that collects the quench water leaving the
bottom of the bed has overflow pipes to direct the condensed water onto
the valve tray (tray #2) below. The quench water collecting on the
chimney tray is pumped by the SWS Quench Water Pump,
A2-GA1522A/B, to the SWS Quench Water Cooler, A2-EC1520, to cool
the water from 99°C [210°F] to 66°C [150°F] to reject the heat removed
from the stripping steam in the quench section of the column. The cooling
rate is adjusted as necessary to control the column overhead temperature
at 85°C [185°F]. This allows the NH3 and H2S stripped from the water to
leave the column at 0.85 kg/cm2(g) [12 PSIG]and flow to the SRUs.
A chimney tray is located below the bottom valve tray to gather all of the
column liquids to feed the Sour Water Stripper Reboiler. The column
section located below this chimney tray serves to separate the outlet
steam and treated water from the reboiler.
The chimney tray gathers the tower liquids to feed the reboiler. The outlet
from the reboiler reenters the column below the chimney tray, with the
vapor produced by the reboiler flowing upward through the chimneys in
order to reach the valve trays above.
stream, so that the hot water leaving the Sour Water Stripper can preheat
the sour water before it feeds the Sour Water Stripper. This cross
exchange saves reboiler duty by preheating the sour water, and reduces
the load on the SWS Bottoms Cooler by partially cooling the hot stripped
water.
the sour water outlet section, where the sour water is pumped to the Sour
Water Tank.
CAUTION
In general, decreasing the quench water circulation rate will increase the
quench water temperature upstream of the cooler (which increases the
corrosion rate) and may increase the Sour Water Stripper Overhead
temperature if the cooler cannot cool the quench water sufficiently. Care
should be taken when reducing the quench water circulation rate to
ensure that the corrosion rate in the quench water circulation loop does
not become excessive.
As the feed rate to the SWS Stripper decreases, the quench water
circulation rate can decrease in proportion with the feed flow rate down to
about 50% of design flow rate. Below this point, the quench water rate
cannot be allowed to drop any further without risking poor performance in
the packed section of the SWS Stripper due to uneven liquid distribution
and wetting of the packing. At lower feed rates (below 50%) simply setting
the quench water flow rate to the column at about 50% of design should
maintain adequate performance. (It should be noted, however, that there
is really no detrimental effect if the quench water circulation is simply left
at the design value at all times. The only drawback is slightly higher
power consumption by the pump and aerial cooler.)
Increasing the quench water temperature will increase the overhead gas
temperature and water content which increases the load on the
downstream SRUs (since water is a product of the Claus reaction, higher
water content in the SWS feed gas can negatively impact the recovery of
in the SRUs). However, decreasing the quench water temperature (and
correspondingly the overhead gas temperature) may lead operating
issues including salt deposition and plugging in the downstream piping
and equipment. Ammonium salts can form in the gas stream leaving the
top of the Sour Water Stripper if the gas temperature falls below about
70°C. These salts can plug the mist eliminator in the top of the Sour Water
Stripper as well as the downstream piping and equipment. In addition,
decreasing the overhead gas temperature below about 82°C may prevent
the ammonia from leaving the top of the column. Instead it may become
“trapped” in the column where it will concentrate, or it may leave in the
stripped water causing the treated water to exceed the specification for
ammonia.
The flow rate and temperatures shown on the Process Flow Diagram are
usually a good compromise between minimizing corrosion, minimizing the
load on the downstream SRUs, and minimizing operating issues within the
SWS unit.
8.6.3 pH Control
High pH water tends to hold H2S in solution and aids in releasing
ammonia from sour water. Conversely, low pH water tends to hold
ammonia in solution and improves the stripping of H2S. By injecting a
small amount of caustic near the tower bottom, ammonia stripping in the
bottom of the Sour Water Stripper can be improved while the H2S is still
stripped in the upper part of the tower.
Injection points for caustic addition have been supplied in the lower
section of the Sour Water Stripper. In the event that the stripped water
cannot meet the low ammonia specification, caustic can be added to the
tower to increase the pH and improve the ammonia stripping in the tower.
If caustic is added, injection control is critical to limit the pH of the stripped
water to about 8.0.
C. Check the rotation of the fans on the SWS Quench Water Cooler and
the SWS Bottoms Cooler, by operating each fan for a short period.
D. Check all piping and equipment to be sure that all blinds have been
removed and that no valves are vented to atmosphere.
F. Check all relief valves to ensure that they are installed in the proper
locations, the inlet and outlet block valves (if provided) are open, the
bypass valves (if provided) are closed, and the relief valves are set
for the correct relieving pressure.
Failure to clean the system properly prior to startup can lead to operating
problems (heat exchanger fouling, rapid filter plugging, etc.).
(1) Set the output from the Sour Water Flash Drum level controller
to 0% to fully close the Sour Water Flash Drum level control
valve.
(2) Set the output from the SWS Inlet flow controller to 100% to
fully open the SWS Inlet flow control valve.
(3) Set the output from the SWS level controller to 100% to fully
open the level control valve.
(4) Set the output from the Quench Water flow controller to 100%
to fully open the Quench Water flow control valve.
(5) Set the output from the SWS Stripper Reboiler steam flow
controller to 0% to fully close the steam flow control valve.
(6) Set the output from the SWS pressure controller to 0% to fully
close the overhead pressure control valve to the SRUs.
C. Verify that the bypass valve on the pressure control valve to the flare
is closed. Open both of the isolation block valves at this control
station.
Water Tank, and fully close the automated valve in the Treated
Water line downstream of the SWS Bottoms Cooler. Visually confirm
that these valves are properly positioned.
F. Verify that the manual block valve at the inlet to the Sour Water Tank
is open.
G. Verify that the manual block valve in the fill line for the Quench Water
Loop is closed.
H. Verify that the SWS Inlet flow control valve is fully open. Open both
of its isolation block valves and its bypass valve.
I. Verify that the SWS level control valve is fully open. Open both of its
isolation block valves and its bypass valve.
J. Verify that the Quench Water flow control valve is fully open. Open
both of its isolation block valves and its bypass valve.
K. Verify that the Sour Water Flash Drum level control valve is fully
closed. (This will prevent water from entering the upstream
equipment if the Sour Water Tank is accidentally over-filled.)
L. The Sour Water Filters will not be used to filter solids during this
time, but the filter vessels and their piping are to be flushed and
cleaned. Remove the filter elements, then bolt-up the filters. Open
the inlet and outlet block valves on the filters, and open the bypass
valve around the filters.
N. Once there is an adequate level in the tank, open the suction valve
on a SWS Feed Pump and use its drain valve to be sure the pump is
flooded with water. Start the pump, then open its discharge valve.
Watch the level in the Sour Water Tank as the pump fills the
downstream piping and begins to fill the Sour Water Stripper. When
the level drops to the low-low level shutdown it should shut down the
pump. If it does not, stop the pump manually before it loses suction
and correct the problem with the low level shutdown before
proceeding.
O. Continue filling the Sour Water Tank with condensate and pumping
the water to the Sour Water Stripper periodically, until the level in the
Stripper is all the way to the top of its level gauge.
Watch the level in the Sour Water Stripper as the pump fills the
downstream piping and begins to circulate back to the Sour Water
Tank. When the level drops to the low-low level shutdown it should
shut down the pump. If it does not, stop the pump manually before it
loses suction and correct the problem with the low level shutdown
before proceeding.
Q. Once circulation is achieved and the level in the Sour Water Stripper
is adequate (about halfway up in the level gauge), discontinue the
addition of condensate.
R. Circulate the water and blow down the low point drains until all of the
drain water is clear. Add more condensate as necessary to maintain
the level in the Sour Water Stripper.
At some point during the washing procedure, the standby SWS Feed
Pump and the standby SWS Bottoms pump should be placed in
service while the other pumps are shut down. This will ensure
cleaning out all pumps and their associated piping.
S. When the drain water begins to clear, open the manual block valve in
the Quench Water fill line, open the suction valve on a SWS Quench
Water Pump and use its drain valve to be sure the pump is flooded
with water. Start the pump, then open its discharge valve.
Watch the level in the Sour Water Stripper as the pump fills the
quench water circulation loop. Add additional condensate to the Sour
Water Tank if necessary and pump the water to the Sour Water
Stripper.
T. Once circulation is achieved in the Quench Water loop and the level
in the Sour Water Stripper is adequate (about halfway up in the level
gauge), discontinue the addition of condensate and close the manual
block valve in the Quench Water fill line.
U. Circulate the water in the Quench Water loop and blow down the low
point drains until all of the drain water is clear.
V. Once the drain water is clear in the main circulation loop and Quench
Water loop, shutdown the pumps and completely drain the system.
Drain the system as quickly as possible, so that the water velocity
helps to flush the solids from all parts of the system.
B. Close the inlet and outlet block valves (but leave the bypass
valves open) on the Sour Water Filters, then install the proper
elements in the filters. Leave the block valves closed on each
filter for now.
E. Start a fan on the SWS Bottoms Cooler and place the bottoms
temperature controller in service with a setpoint of 60°C.
G. Open the high point vent valve on the Stripper overhead line
and allow the steam to purge any air from the vessel. As the
pressure builds, the vent valve can be closed.
J. Ensure that the fans are running on the SWS Bottoms Cooler
and the SWS Quench Water Cooler.
K. If the control loops for the Sour Water Stripper have not already
been placed in service, do so at this time. Switch the SWS
level controller, and the SWS Inlet flow controller in the DCS to
"automatic" with their setpoints set to their normal values.
(2) "Crack" the filter inlet block valve open slightly and allow
the filter to fill with sour water. When the filter is full, close
its vent valve.
(3) Open the inlet and outlet block valves on the filter.
(4) Slowly close the valve in the bypass line around the filter.
Note: At this point the sour water system is ready for service. It
can remain in this operating mode indefinitely while the
rest of the Complex is prepared for startup. Check the
system periodically for indications of plugging, etc. (low
flow, erratic pump discharge pressure, high filter pressure
drop), as solid materials may accumulate at various points
in the system over time.
Watch the level in the Sour Flash Drum as the pump fills the
downstream piping and begins to flow to the Sour Water Tank.
When the level drops to the low-low level shutdown it should
shut down the pump. If it does not, stop the pump manually
before it loses suction and correct the problem with the low
level shutdown before proceeding.
O. Place the Sour Water Flash Tank level controller in the DCS in
“automatic” and set its setpoint to its normal value.
The sour water will continue to circulate from the Sour Water Tank to
the Sour Water Stripper and back to the tank. The Sour Water Tank
is large enough to provide 3-4 days of residence time for the
produced sour water in the event the Sour Water System is not ready
to export treated water at this time.
The Sour Water Stripper pressure controller will now take over
control of the Sour Water Stripper pressure by opening the
pressure valve to send the acid gas to the SWS Gas Knock-Out
Drums in the SRUs. The Sour Water Stripper pressure
controller to the flare will close the acid gas pressure valve and
stop the flow of acid gas to the flare. If the SRUs shut down (or
some other upset causes the Sour Water Stripper pressure to
rise), the Sour Water Stripper pressure controller to the flare will
act as an over-ride and divert the acid gas to the flare.
(2) The steam heating systems are in service and the level
control on the Reboiler condensate pot is functioning
properly.
(1) Set the output from the SWS Inlet flow controller to 100%
to fully open the SWS Inlet flow control valve.
(2) Set the output from the SWS level controller to 100% to
fully open the level control valve.
(3) Set the output from the Quench Water flow controller to
100% to fully open the Quench Water flow control valve.
C. Confirm that the output from the SWS Stripper Reboiler steam
flow controller is set to 0% and the steam flow control valve is
fully closed.
D. Confirm that the output from the SWS pressure controller is set
to 0% and the overhead pressure control valve to the SRUs is
fully closed.
F. Verify that the bypass valve on the pressure control valve to the
flare is closed and that both of the isolation block valves are
open.
H. Verify that the manual block valve at the inlet to the Sour Water
Tank is open.
I. Verify that the manual block valve in the fill line for the Quench
Water loop is closed.
Watch the level in the Sour Flash Drum as the pump fills the
downstream piping and begins to send sour water to the Sour
Water Tank. When the level drops to the low-low level
shutdown it should shut down the pump. If it does not, stop the
pump manually before it loses suction and correct the problem
with the low level shutdown before proceeding.
Watch the level in the Sour Water Tank as the pump fills the
downstream piping and begins to fill the Sour Water Stripper.
Watch the level in the Sour Water Stripper as the pump fills the
quench water circulation loop. If the level in the stripper falls
below the low level alarm point, stop the SWS Quench Water
Pump and pump additional sour water to the Stripper from the
Sour Water Tank to bring the level in the level back up before
restarting the SWS Quench Water Pump.
Q. Start a fan on the SWS Bottoms Cooler and place the bottoms
temperature controller in service with a setpoint of 60°C.
U. Ensure that the fans are running on the SWS Bottoms Cooler
and the SWS Quench Water Cooler.
V. If the control loops for the Sour Water Stripper have not already
been placed in service, do so at this time. Switch the Sour
Water Flash Tank level controllers, the SWS level controller,
and the SWS Inlet flow controller in the DCS to "automatic" with
their setpoints set to their normal values.
The sour water will continue to circulate from the Sour Water Tank to
the Sour Water Stripper and back to the tank. The Sour Water Tank
is large enough to provide 3-4 days of residence time for the
produced sour water in the event the Sour Water System is not ready
to export treated water at this time.
The Sour Water Stripper pressure controller will now take over
control of the Sour Water Stripper pressure by opening the
pressure valve to send the acid gas to the SWS Gas Knock-Out
Drums in the SRUs. The Sour Water Stripper pressure
controller to the flare will close the acid gas pressure valve and
stop the flow of acid gas to the flare. If the SRUs shut down (or
some other upset causes the Sour Water Stripper pressure to
rise), the Sour Water Stripper pressure controller to the flare will
act as an over-ride and divert the acid gas to the flare.
(2) The steam heating systems are in service and the level
control on the Reboiler condensate pot is functioning
properly.
A. Slowly reduce the output from the Treated Water hand control in the
DCS is to 0% output to fully open the automated valve in the
Startup/Re-run line to the Sour Water Tank, and fully close the
automated valve in the Treated Water line downstream of the SWS
Bottoms Cooler. Visually confirm that these valves are properly
positioned.
B. Place the stream flow controller in manual and set its output to 0% to
close the stream flow control valve and stop the steam flow to the
Sour Water Stripper Reboiler.
C. Continue to circulate the sour water and operate the SWS Bottoms
Cooler and the SWS Quench Water Cooler until the sour water is
cool.
D. Once the sour water is cool, shut down the SWS Feed Pump to stop
the flow of sour water to the Sour Water Stripper and close the block
valves in the pump suction lines.
E. Place the SWS flow controller in the DCS in "manual" and set its
output to 0% to fully close the sour water inlet flow control valve.
F. Shutdown the SWS Quench Water Pumps and shut down the fans
on the SWS Quench Water Cooler.
G. Place the quench water flow controller in the DCS in "manual" and
set its output to 0% to fully close the quench water flow control valve.
H. Use the SWS Bottoms pump to pump the sour water from the Sour
Water Stripper to the Sour Water Tank until the low-low level
shutdown is activated. This should shut down the SWS Bottoms
Pump. Monitor the level in the Sour Water Stripper and be prepared
to shut down the pump if the low-low level shutdown fails to activate.
I. Place the SWS level controller in the DCS in "manual" and set its
output to 0% to fully close the SWS level control valve.
K. Drain the remaining sour water in the SWS equipment to the Closed
Drain System.
L. Verify that the SWS level control valve is fully closed. Close both of
its isolation block valves and its bypass valve.
M. Verify that the SWS flow control valve is fully closed. Close both of
its isolation block valves and its bypass valve.
N. Verify that the quench water flow control valve is fully closed. Close
both of its isolation block valves and its bypass valve.
O. The SWS is now ready to be isolated and made safe for entry.
Table of Contents
9. SULFUR RECOVERY .................................................................................................. 9-4
9.1 PURPOSE OF SYSTEM ....................................................................................... 9-4
9.2 SAFETY ................................................................................................................. 9-4
9.3 PROCESS DESCRIPTION.................................................................................... 9-5
9.3.1 Overview......................................................................................................... 9-5
9.3.2 General ........................................................................................................... 9-6
9.3.3 Feed Gas Processing ..................................................................................... 9-6
9.3.4 Thermal Processing........................................................................................ 9-7
9.3.5 Catalytic Processing ....................................................................................... 9-8
9.3.6 Air Control System.......................................................................................... 9-9
9.3.7 Molten Sulfur Handling ................................................................................. 9-10
9.3.8 Steam Production ......................................................................................... 9-10
9.4 EQUIPMENT DESCRIPTION .............................................................................. 9-11
9.4.1 Reactor Furnace, A2-BA1530 (A2-BA1540) ................................................. 9-11
9.4.2 Acid Gas Burner Assembly, A2-BA1531 (A2-BA1541) ................................ 9-12
9.4.3 Acid Gas Knock-Out Drum, A2-FA1530 (A2-FA1540) ................................. 9-12
9.4.4 SWS Gas Knock-Out Drum, A2-FA1531 (A2-FA1541) ................................ 9-12
9.4.5 Reactor, A2-DC1530 (A2-DC1540) .............................................................. 9-13
9.4.6 Catalyst for Sulfur Plant Reactors, A2-MC1530 (A2-MC1540) ..................... 9-13
9.4.7 Acid Gas Preheater, A2-EA1530 (A2-EA1540) ............................................ 9-13
9.4.8 Sulfur Condenser, A2-EA1531 (A2-EA1541) ............................................... 9-13
9.4.9 Reactor No. 1 Feed Heater, A2-EA1532 (A2-EA1542) ................................ 9-14
9.4.10 Reactor No. 2 Feed Heater, A2-EA1533 (A2-EA1543) ................................ 9-14
9.4.11 Reactor No. 3 Feed Heater, A2-EA1534 (A2-EA1544) ................................ 9-15
9.4.12 Sulfur Surge Tank, A2-FB1530 (A2-FB1540) ............................................... 9-15
9.4.13 Acid Gas Knock-Out Drum Pump, A2-GA1530A/B (A2-GA1540A/B) .......... 9-16
9.4.14 SWS Gas Knock-Out Drum Pump, A2-GA1531A/B (A2-GA1541A/B) ......... 9-17
9.4.15 Sulfur Storage Tank Vent Ejector, A2-EE1530 (A2-EE1540) ....................... 9-17
9.4.16 Process Air Blower, A2-GB1530A/B (A2-GB1540A/B)................................. 9-18
9.4.17 Air Blower Suction Screen/Silencer, A2-FD1530A/B (A2-FD1540A/B) ........ 9-19
9.4.18 Process Air Vent Silencer, A2-FG1530A/B (A2-FG1540A/B) ....................... 9-19
9.4.19 Sulfur Drain Seal Assembly, A2-ME1530A-D (A2-ME1540A-D) .................. 9-19
9.4.20 Refractory for Reactor Furnace and Waste Heat Boiler, A2-MR1530
(A2-MR1540) .............................................................................................................. 9-20
9.4.21 Ceramic Ferrules for Waste Heat Boiler, A2-MR1532 (A2-MR1542) ........... 9-20
9.4.22 Refractory for Waste Heat Boiler, A2-MR1533 (A2-MR1543) ...................... 9-20
9.4.23 Refractory for Sulfur Condenser, A2-MR1534 (A2-MR1544) ....................... 9-20
9. SULFUR RECOVERY
9.1 Purpose of System
The purpose of the Sulfur Recovery Units (SRUs) is to dispose of H2S-laden
acid gas. This gas is produced by the new Amine Regeneration Unit and Sour
Water Stripping Unit. Acid gases of this type are not allowed into the
atmosphere, as they are highly toxic. If burned in a flare system, the pollutants
would exceed emission standards. Each Sulfur Recovery Unit can take enough
H2S out of the acid gas so that the remaining tailgas can be processed in a
Tailgas Cleanup Unit to meet the emission standards after incineration. Also,
the byproduct of pure sulfur is a marketable product.
9.2 Safety
WARNING
The acid gases produced by the new Amine Regeneration Unit (ARU) and
the new Sour Water Stripping Unit (SWS) are routed to two parallel Claus
Sulfur Recovery Units (SRUs) using technology licensed from BP Amoco
Corporation. The H2S is converted into molten elemental sulfur and
routed to the common Sulfur Degassing Unit (SDU) that uses technology
licensed from BP Amoco Corporation to reduce the H2S content of the
sulfur to less than 10 PPMW. The combined tailgas from the sulfur plants
is processed in a Tailgas Cleanup Unit (TGCU) using the Shell Claus
Off-gas Treating (TGCU) process licensed by Shell Global Solutions (US)
Inc. to produce an acid gas stream that is recycled back to the Claus plant
so that the overall sulfur recovery is 99.9 wt. % or better.
The two process trains are identical, so all of the information that follows
applies to both trains. Where references to equipment or instrument tag
numbers are given, the SRU Train 1 tag number is given first followed by
the SRU Train 1 tag number in parentheses.
9.3.2 General
Each sulfur plant processes 1,181 Nm3/H of acid gas from the Amine
Regeneration Unit and 33 Nm3/H of off-gas from Sour Water Stripping
(SWS) Unit, plus 50% of the recycle acid gas from the Tailgas Cleanup
Unit. Each sulfur plant will recover 94-96% of the sulfur contained in the
total acid gas feed as elemental sulfur, producing about 34.6 MT/D of
molten sulfur product. The tailgas leaving each sulfur plant is routed to
the common TGCU.
The sulfur plant contains one non-catalytic conversion stage and three
catalytic conversion stages in series. The Claus reaction is highly
exothermic, releasing a great deal of heat energy that is recovered as HP
and LP steam in heat exchangers following the conversion stages.
SWS gas from the Sour Water Stripping Unit is routed to the SWS Gas
knock-Out Drum, A2-FA1531 (A2-FA1541), at 85°C [185°F] and
0.70 kg/cm2(g) [10.0 PSIG]. Entrained liquids are separated and
automatically routed back to the Sour Water Flash Drum by the SWS Gas
Knock-Out Drum Pump, A2-GA1531A/B (A2-GA1541A/B), on start/stop
level control. The scrubbed SWS gas mixes with the majority of the
preheated amine acid gas and flows to the Acid Gas Burner, A2-BA1531
(A2-BA1541). The remainder of the amine acid gas is routed into the
sides of the Reactor Furnace, A2-BA1530 (A2-BA1540), on flow ratio
control to ensure proper destruction of the ammonia in the first zone of the
furnace as described below.
The combustion products pass into the first combustion zone of the
Reactor Furnace, which provides the necessary residence time to allow
these reactions to reach equilibrium. At 1370°C [2500°F] or above (with
the proper residence time), ammonia is almost completely destructed to
nitrogen and water. The first combustion zone is controlled at or above
this temperature by adjusting the amount of amine acid gas bypassing the
burner. Combustion of the SWS gas at or above this temperature in a
reducing atmosphere is essential for destruction of the ammonia, and
avoids formation of undesirable and troublesome compounds such as
sulfur trioxide.
The first combustion zone of the Reactor Furnace is separated from the
second zone by a refractory checker wall. The amine acid gas bypassing
the burner is injected into the Reactor Furnace immediately downstream
of the checker wall, where it mixes with the burner effluent. The second
zone is large enough to provide sufficient residence time for the
The effluent from the Reactor Furnace enters the tubes in the Waste Heat
Boiler, A2-BF1530 (A2-BF1540), where the gas is cooled to 328°C
[622°F] by producing HP steam. The gas is then routed through the first
condensing pass of the Sulfur Condenser, A2-EA1531 (A2-EA1541), and
further cooled to 165°C [329°F] by producing LP steam. The outlet
channel of the Sulfur Condenser is extended and contains a compartment
that serves as a separator for the condensed sulfur that is formed as the
gases are cooled. About 65% of the sulfur entering the sulfur plant is
recovered as condensed liquid sulfur here.
In this first catalytic conversion stage, the majority of the remaining sulfur
compounds are converted to elemental sulfur vapor by reaction (2). In
addition, much of the organic sulfur compounds formed by side reactions
in the Reactor Furnace, carbonyl sulfide (COS) and carbon disulfide
(CS2), are hydrolyzed back to H2S in this catalyst bed. Hydrolysis of the
organic sulfur compounds helps achieve high sulfur recovery by
converting the organic sulfur compounds into sulfur species that will react
via the Claus reaction to produce sulfur. Special promoted catalysts are
often employed for higher COS/CS2 conversion, and this catalytic stage is
often operated at higher temperatures since this also increases
conversion.
The sulfur vapor produced the first catalyst bed is then condensed at
about 161°C [322°F] in the second condensing pass of the Sulfur
Condenser by generating additional LP steam. About 20% of the inlet
sulfur is condensed and recovered as liquid sulfur in the separator
chamber at the outlet of this condenser pass. The vapor from the second
condensing pass is reheated to 210°C [410°F] using HP steam in the
Reactor No. 2 Feed Heater, A2-EA1533 (A2-EA1543), and is routed to the
The vapor leaving the third condensing pass is reheated to 204°C [400°F]
using HP steam in the Reactor No. 3 Feed Heater, A2-EA1534
(A2-EA1544), and flows to the third catalyst chamber in the Reactor, the
final conversion stage. More conversion occurs in this third catalytic stage
before the gas is cooled in the fourth pass of the Sulfur Condenser by
generating additional LP steam. An additional 2% of the total sulfur is
recovered in the separator chamber at the outlet of this fourth and final
condensing pass, bringing the total sulfur recovery to approximately 94%
in the Claus sulfur plant. The remaining vapor leaves the fourth pass of
the Sulfur Condenser at about 156°C [313°F] and flows to the TGCU.
The amine acid gas flow rate and SWS gas flow rate (and fuel gas flow
rate, if any) are measured, summed together, and sent to the ratio
controller which adjusts the air flow, yielding feed-forward control that
allows the sulfur plant to compensate for changes in the amine acid gas
and SWS gas flow rates (and the fuel gas flow rate, also).
The H2S:SO2 ratio of the gas from the fourth condensing pass of the
Sulfur Condenser is continuously analyzed by the air demand analyzer.
This analyzer signal is then used to change the setpoint of the flow ratio
controller, thus providing feed-back control to allow the sulfur plant to
adjust to variations in amine acid gas and/or SWS gas composition,
temperature, and pressure.
The Sulfur Surge Tank provides storage for about 160 metric tons of raw
sulfur production from the sulfur plant. The Sulfur Surge Tank is a
horizontal cylindrical tank resting in a concrete vault. The tank is
constructed of carbon steel and is equipped with internal steam coils. The
Sulfur Surge Tank Vent Ejector, A2-EE1530 (A2-EE1540), uses HP
motive steam to route the tank vapors to the Tailgas Thermal Oxidation
system.
Low pressure steam at 4.2 kg/cm2(g) [60 PSIG] is produced in the Sulfur
Condenser. Part of this steam is used to preheat the amine acid gas, heat
the Sulfur Storage Tank, heat the steam-jacketed lines, and for steam
tracing services. The remainder is routed to the complex's LP steam
header.
The four sets of condensing pass tubes are immersed in the water-filled
section of the shell, allowing them to cool the hot gases leaving the Waste
Heat Boiler and the three catalyst beds in the Reactor. The boiling water
in the shell of the exchanger cools the gases and condenses sulfur from
the process streams. The steam produced will be controlled at about
The boiler is equipped with level transmitters that will shut down the SRU
should the water level fall to within 75 mm of the top row of condensing
tubes. The shutdown requires that 2 out of 3 transmitters have a low-low
level indicated. Operation of the boiler without a sufficient water level
could possibly damage the tubes.
The primary ventilation system for the Sulfur Storage Tank is the Sulfur
Surge Tank Vent Ejector, A2-EE1530 (A2-EE1540). It uses HP steam as
the motive force to circulate air through the tank. Ambient air enters
through the breather vents at each end of the tank and is educted to the
ejector suction. The discharge from the ejector is routed to the TTO for
disposal. This air circulation dilutes the H2S that "weathers off" from the
liquid sulfur so that the concentration remains below the lower explosive
limit. The circulation also prevents accumulation of water in the tank that
could cause rapid corrosion.
sweeps through the tank before entering the vent stack. The
steam-jacketing on the vent stack heats the air in the stack, providing the
natural-draft driving force that makes the system work.
WARNING
WARNING
WARNING
WARNING
CAUTION
The seals are fully steam-jacketed and designed to be installed in the top
of the Sulfur Surge Tank. Each seal has a hinged inspection hatch to
allow observation and sampling of the flow from each condenser pass.
The liquid sulfur from the inspection basin flows down to the bottom of the
Sulfur Surge Tank through a drain pipe to prevent free-fall of the liquid
sulfur, which could cause static electricity to build up. The drain seals are
mostly carbon steel, except for the inspection hatches which are
aluminum.
Each drain seal has removable blind flanges to allow "rodding" its
rundown line and its dip leg. Before removing either flange, close the
block valve in the rundown line to prevent the escape of process gas to
the surroundings when the plugging is cleared. When the rodding
operation is complete and the flange(s) are back in place, remember to
reopen the block valve.
Most of the steam produced by the Waste Heat Boiler is routed to the
Thermal Oxidizer Waste Heat Boiler, A2-BF1570, to be superheated
before it is exported to the HP Steam header. The remaining portion of
this steam is withdrawn and directed to the three heaters for the Reactor
feeds, the Reactor No. 1 Feed Heater, the Reactor No. 2 Feed Heater,
and the Reactor No. 3 Feed Heater, which operate in a thermosiphon loop
with the Waste Heat Boiler. The steam flows over and condenses on the
outside of the tubes in these exchangers, heating the gas within the tubes
to raise the temperatures of the gas streams to the desired feed
temperatures for the catalyst beds. The condensate from these three
exchangers returns to the Waste Heat Boiler by gravity flow.
The boiler is equipped with level transmitters that will shut down the SRU
should the water level fall to within 75 mm of the top row of tubes. The
shutdown requires that 2 out of 3 transmitters have a low-low level
indicated. Operation of the boiler without a sufficient water level will result
in severe damage to the tubes and the shell.
WARNING
The feed-forward portion of the control loop uses the acid gas and fuel
gas flow rates to compute the setpoint for the air flow controller,
A2-FIC15370. Since the amine acid gas, SWS gas, and fuel gas require
different amounts of air, the three flow rates are metered separately and
then summed by A2-FY15345 and A2-FY15349. The three signals are
also biased (by A2-FY15320, A2-FY15331, and A2-FY15355) to allow for
the differences in air requirements. In this manner, the setpoint for
A2-FIC15370 will be properly adjusted as the individual gas flow rates
vary.
A special photometric analyzer samples the process gas in the sulfur plant
tailgas to determine the relative amounts of H2S and SO2 in the gas. The
analyzer provides an output signal that is proportional to the amount the
air flow rate must change in order to bring the H2S:SO2 ratio to the
optimum 2:1 value. This signal is the feed-back part of the control loop,
and is used to make minor adjustments to the air:acid gas ratio and allow
the control system to respond to compositional variations in one or more
of the acid gas feeds.
The control loop is discussed in detail in the sections that follow. The
discussions are divided into five sections: air requirement computation for
the acid gas streams, air:acid gas ratio adjustment, air requirement
computation for fuel gas, air flow control, and local/remote control.
The two bias calculation blocks multiply each gas flow rate by a gain
factor equal to the process air required per unit of flow for that
stream. The appropriate gain factors are 2.563 Nm3/Nm3 for the
amine acid gas (A2-FY15320) and 2.186 Nm3/Nm3 for the SWS gas
(A2-FY15331). A2-FY15345 then sums the two outputs from the
bias relays, providing an output that (at design conditions) is equal to
the required air flow rate for the acid gas streams. This output is
then supplied to the ratio adjustment relay, A2-AY15348. These
factors can be revised periodically if changes in feedstocks, etc.
cause long-term changes in the compositions of one or both of the
acid gas streams.
Note that each bias relay has a "zero" switch (A2-HS15320 for
A2-FY15320 and A2-HS15331 for A2-FY15331). These switches
can be used to "turn off " their respective relays when there is no flow
of the corresponding gas stream. This prevents an erroneous
reading from a flow transmitter causing errors in the theoretical air
flow computations. A similar switch (A2-HS15356) is included for the
fuel gas bias relay (A2-FY15355) discussed in Section 9.5.1.3.
The fuel gas flow rate is linearized and input to the DCS by
A2-FT15355. Flow controller A2-FIC15355 in the DCS converts this
linear signal into a flow rate in engineering units. Bias relay
A2-FY15355 then multiplies the fuel gas flow rate by the appropriate
gain factor for this fuel gas, 32.509 Nm3/Nm3 (For the C4 LPG), to
give the computed air flow for the fuel gas. This is added to the
corrected air flow for the acid gas streams by summing relay
A2-FY15349, giving the total air flow rate that is then supplied to the
air flow controller, A2-FIC15370, as a remote setpoint.
(2) Once the pilot burner in the Acid Gas Burner has been lit and
the SRU is ready to accept acid gas (furnace up to temperature,
etc.), the Warmup Bypass Valves must be closed before acid
gas can be introduced into the SRU. However, in order to avoid
activating the "complete flowpath interlock" alarm and possibly
tripping the Reactor Furnace high-high pressure S/D, there
must be an open flowpath through the SRU before the bypass
valves are closed.
close the two bypass valves and initiate the nitrogen purge,
A2-HV15453, between the two valves. By automating the valve
switching steps and including checks of the limits switches in
the logic, the chance of accidentally causing an SRU1 ESD due
to over-pressure during startup are greatly reduced.
then open the valve in its purge gas supply to begin purging the
burner. For the pilot burner, the block valve in its air supply is also
closed and the ignition system, A2-BX15368, is de-energized.
If the burner is "off " (and the "flame proven" is already satisfied by
one of the other burner tips), pressing its push-button will ignite the
burner by closing the valve in its purge gas supply to cease purging
the burner, and closing the vent valve and opening the two block
valves in its fuel gas supply. For the pilot burner, the block valve in
its air supply is also opened and its ignition system, A2-BX15368, is
energized for 15 seconds.
3. As the output drops below 66.7%, the suction valve will not close
any further (to prevent starving the blower for air), the discharge
valve will continue to throttle, and the blow-off valve will begin to
open and vent part of the air to the atmosphere instead of flowing to
the process.
The output signals from the DCS to each of the control valves should
be displayed on the DCS console. The I/P transducers mounted on
the valves in the field are direct (i.e., 4-20 mA to the transducer gives
an output of 0-100% from the valve positioner).
The split-range values on the P&IDs are the suggested initial settings
for the control schemes on these blowers. These values may need
adjustment once the SRUs are placed in operation, depending on
the operating characteristics of each particular air blower and its
control valves. These adjustments can be made during plant startup.
Once all of the control signal is going to the off-line blower and none
is going to the on-line blower, the off-line blower has become the
on-line blower. What was the on-line blower is now the off-line
blower, and it can then be shut down without affecting the SRU.
b. There is always the potential to have acid gas in the process air
piping, so having the blower suction and blow-off valves open
while its blower is not running should be minimized to reduce
the risk of releasing acid gas to the atmosphere. When the
operator presses the "permit to start" push-button,
A2-HPB15338A/B, for a blower, its suction and blow-off valves
will open for 30 seconds to allow time for the operator to start
the blower using the local start/stop control.
If the blower is not started within this time, the suction and
blow-off valves are closed and the "permit to start" is disabled.
The operator will have to press A2-HPB15338A/B again before
the blower can be started.
c. If the operator starts the blower and the motor starter contacts
for the blower indicate that the blower is running within this
time, the solenoid valve on the blower discharge valve is then
energized so that the operator can increase the control signal to
the blower to open the discharge valve and commence air flow
to the process.
For a simplified example, consider the case where there is no SWS acid
gas flow. Without any amine acid gas bypassed, only 33% of the H2S at
the burner would be burned. If one-third of the total amine acid gas
bypasses the burner, then 50% of the H2S in the amine acid gas sent to
the burner must be burned in order to convert one-third of the total H2S to
SO2. Thus, a larger fraction of the H2S entering the burner is combusted
when part of the acid gas bypasses the burner, which raises the flame
temperature.
The furnace temperature control loop for the Train 1 SRU consists of: the
optical pyrometer, A2-TT15375; the Reactor Furnace temperature
controller, A2-TIC15375; the acid gas bypass flow ratio controller,
A2-FFIC15350; the acid gas valve to the burner, A2-FV15351, and the
acid gas bypass valve, A2-FV15350. (Note that an optical pyrometer
does not actually measure temperature. Instead, it infers the furnace
temperature by measuring the infrared radiation inside the Reactor
Furnace. Experience has shown that the temperature indicated by an
When the Train 1 SRU is operating at low flow rates, there may not be
enough pressure drop in its Acid Gas Burner to give good control of the
bypass acid gas with A2-FV15350. For this reason A2-FV15351 is
designed to work together with A2-FV15350 over split ranges of the
A2-FFIC15350 controller output. If A2-FV15350 goes fully open at lower
flow rates, the controller output will continue to increase so that
A2-FV15351 begins to "throttle" in the amine acid gas line to the burner
and force more of the acid gas to flow through A2-FV15350.
The local H-O-A switches near the pumps allow the operator to place
these pump in "auto" start mode. The DCS should start the pump when
the liquid level reaches the "pump start" level in the drum. After the liquid
is pumped out, the DCS should stop the pump when the level reaches the
"pump stop" level. If the pump fails to start, or the liquid level is rising
faster than the pump can keep up with, the DCS should give a LAH. If the
level continues to rise, the PLC will activate the SRU ESD system when
the level reaches the LAHH setpoint to prevent carry-over of liquids into
the Acid Gas Burner and the Reactor Furnace. If the pump fails to stop,
the DCS should give a LAL.
Similarly, little (if any) liquid will drop out in the SWS Gas Knock-Out
Drum, A2-FA1531 under normal conditions. It can also have liquids
accumulate rapidly during an upset, however, so the SWS Gas Knock-Out
Drum Pump, A2-GA1531A/B has also been designed to automatically
start and stop as required by the liquid level in the drum, based on the
level signal sent to the DCS. Level signals are provided to the PLC by
three LTs for use as a 2oo3 voting shutdown.
The local H-O-A switches near the pumps allow the operator to place
these pumps in "auto" start mode. The DCS should start the pump when
the liquid level reaches the "pump start" level in the drum. After the liquid
is pumped out, the DCS should stop the pump when the level reaches the
"pump stop" level. If the pump fails to start, or the liquid level is rising
faster than the pump can keep up with, the DCS should give a LAH. If the
level continues to rise, the PLC will close the SWS gas inlet valve when
the level reaches the LAHH setpoint to prevent carry-over of liquids to the
Acid Gas Burner. If the pump fails to stop, the DCS should give a LAL.
long as power is restored before the blower "spins down" too much. The
rotors in Process Air Blowers have relatively large moments of inertia so it
takes a relatively long time (usually many seconds) for the rotational
speed to decline to the point that the air flow drops enough to extinguish
the flame in the associated burner.
In order for the blowers to "ride-through", the motor starter circuit must
include an auxiliary contact that is held-in during a power outage, so that if
power is restored the starter contactor will re-engage. The generic motor
starter schematic below shows one way of accomplishing the
"ride-through".
There is a "run permissive" contact from the PLC in the main power
supply to the starter circuit. If the unit ESD is activated for any reason
("flame failure", for instance), this contact opens so that the blower is
There is a "ride-through" contact from the PLC that parallels the usual
"m" latch relay in the starter circuit. The PLC closes this contact when it
receives the "run" status from the blower. If power is restored before the
ESD is activated, this closed contact allows the starter contact to
re-engage and restore the "m" latch to keep the motor going.
Within the PLC logic for each ESD system, the "run" status for each
blower is connected to a TDO (time delay off) timer set for 10 seconds.
Normally-open contacts from the TDO are used in the PLC logic that
determines whether a particular blower is running, as well as the logic that
determines whether any blowers are running. Thus, if power is lost to a
blower and the starter contactor disengages, the TDO contacts will
continue to maintain the "blower running" logic as "true" for up to
10 seconds. If power is restored to the blower within this time and the
starter contactor re-engages, the ESD logic will remain satisfied and the
unit will not shut down. If power is not restored to the blower within this
time, the TDO contacts will open and cause the "blower running" logic to
become "false" and activate the unit ESD.
While the TDO timer is running, all of the unit shutdowns besides "no
blower running" are still active. If any of these other shutdowns are
tripped, the ESD will be activated immediately to shut down the unit. For
example, if the flame is lost in the burner during this time, "flame failure"
will activate the ESD and the unit will shut down immediately. Among
other things, the ESD will then remove the "run permissive" from the
blowers so that the blowers cannot restart.
The logic for an air blower "run permissive" is similar to the ESD logic for
that ESD system, but there are a couple of key differences. First, each
unit ESD includes all of the shutdowns, while the "run permissive" does
not include the "no blower running" or "flame failure" S/Ds to allow starting
an air blower in the first place. Second, the unit ESD requires that the
"MANUAL RESET" push-button be pressed to reset the unit ESD, but the
(1) The outside operator notifies the DCS operator that he is preparing
to test shutdown level transmitter "A" on the Waste Heat Boiler.
(2) The DCS operator confirms that A2-LI15401B and A2-LI15401C are
both indicating adequate level in the boiler, then notifies the outside
operator to proceed.
CAUTION
(3) After being notified to proceed by the DCS operator, the outside
operator blocks-in A2-LT15401A by closing its block valves, then
opens the drain valve on the bottom of the transmitter to drain the
water from the instrument.
(4) If the transmitter is operating properly, the DCS will alarm that there
is a low level in the Waste Heat Boiler on A2-LI15401A. The DCS
operator acknowledges the alarm on the DCS and reports it to the
outside operator.
(5) After being notified of the alarm, the outside operator closes the drain
valve on A2-LT15401A, slowly opens its bottom block valve to allow
the transmitter to fill with water then opens its top block valve. This
should clear the low level alarm on A2-LI15401A in the DCS.
(6) After confirming that the low level alarm has cleared, the other level
transmitters can be tested in a similar fashion.
NOTE: The DCS operator must not begin another task until confirming
that the low level alarm has cleared. This is to guard against
having a level transmitter malfunction that causes an SRU ESD
when the other transmitters are tested.
9.5.8.1 Causes
Any one of the causes listed below will activate the SRU1 ESD
system:
Dual flame scanners are aimed to observe the flames from the
pilot, warmup, and main acid gas burners. If neither scanner
detects a flame (2oo2), a "flame failure" occurs and activates
the SRU1 ESD system. If only one scanner detects a flame
(1oo2), a malfunction alarm is activated in the DCS, but the
SRU1 ESD system is not activated. A third flame scanner,
A2-BY15368, is furnished with the pilot to detect its flame, but it
is used only to activate its status light (A2-GL15368) on the
local Train 1 SRU control panel and a status indicator
(A2-BL15368) in the DCS.
Amine acid gas or SWS gas should not be fed to the Train 1
SRU if its warmup bypass line to the TTO is in use. Otherwise,
very high concentrations of H2S would be sent to the TTO,
possibly leading to a high-high temperature S/D of the TTO and
venting of un-combusted H2S to the atmosphere. The "closed"
limit switches on the warmup bypass valves (A2-HV15441 and
A2-HV15454) must indicate that at least one of these valves is
closed, or the SRU1 ESD system will be activated.
Once the pre-ignition steps have been completed and the BMS
gives a "PERMIT TO IGNITE" for the pilot burner in the Acid Gas
Burner (signaled by illuminating status indicator light
A2-AL15394 on the local Train 1 SRU control panel), an ignition
safety interlock timer is started in the BMS. If an ignition
attempt is not made within 5 minutes, the SRU1 ESD system
will be activated to shut down the sulfur plant. This prevents a
potentially unsafe condition from persisting, where a leaking
fuel gas valve could cause an explosive mixture to form in the
Reactor Furnace, since the air flow is low at this point in the
startup procedure.
9.5.8.2 Effects
An SRU1 ESD shutdown, activated either manually or automatically,
has the following effects on the Train 1 Sulfur Recovery Unit:
a. Shuts off the amine acid gas flow to the Acid Gas Burner by
closing the acid gas shutdown valve, A2-HV15320.
b. Shuts off the SWS gas flow to the Acid Gas Burner by closing
the SWS gas shutdown valve, A2-HV15331.
(1) Shuts off and depressurizes the main fuel gas supply by
closing block valves A2-NV15357 and A2-NV15359 and
opening vent valve A2-NV15358.
(2) Shuts off the pilot air supply by closing block valve
A2-NV15367.
(3) Shuts off and depressurizes the pilot fuel gas supply by
closing block valves A2-NV15363 and A2-NV15365 and
opening vent valve A2-NV15364.
h. Sends the Train 1 SRU S/D status to the TGCU ESD system.
(The TGCU ESD system will shut down the TGCU if neither
SRU is running and the TGCU is not in "startup" mode.)
When the amine acid gas flow to the Train 1 SRU is blocked, the
pressure control system on the stripper in the upstream ARU should
automatically divert acid gas to the flare as required. When the SWS
gas flow to the Train 1 SRU is blocked, the pressure control system
on the stripper in the upstream SWS should also automatically divert
SWS gas to the flare as required.
By leaving the air blower running when a fuel gas flame is lost,
fewer blower restarts are necessary while re-lighting the burner,
resulting in less "wear and tear" on the large motors driving
these blowers.
During warmup while the Train 1 SRU is firing on fuel gas, loss
of the fuel gas supply would cause the fuel gas pressure to
drop. This device will shut off the fuel gas to the Acid Gas
Burner before flame instability creates the potential for an
explosion. The shutdown setpoint is 0.35 kg/cm2(g).
Note that if the Train 1 SRU is firing on acid gas, the transmitter
only activates the Train 1 SRU Fuel gas Burner Shutdown
system (pilot fuel gas and main fuel gas), so the Train 1 SRU
will continue running on acid gas. If, however, the Train 1 SRU
is firing only fuel gas (as indicated by its acid gas firing selector
switch, A2-HS15315, being set to "DISABLED"), the SRU1 ESD
system is activated and the low-low pressure is reported to the
"first out" alarm logic. Example logic to accomplish this is shown
below:
Note that if the Train 1 SRU is firing on acid gas, the transmitter
only activates the Train 1 SRU Fuel gas Burner Shutdown
system (pilot fuel gas and main fuel gas), so the SRU will
continue running on acid gas. If, however, the Train 1 SRU is
firing only fuel gas (as indicated by its acid gas firing selector
switch, A2-HS15315, being set to "DISABLED"), the SRU1 ESD
system is activated and the high-high pressure is reported to
the "first out" alarm logic, as shown by the example logic for the
previous item.
(3) Its manual tailgas block valve and its Tailgas Valve to the
TGCU, A2-HV15462, are both fully open and the TGCU
Complete Flowpath Interlock is satisfied, allowing the
tailgas to flow through the TGCU and then to the TTO.
logic will not be satisfied for the Train 1 SRU. For this reason,
there is a "slow transfer over-ride" switch in the DCS,
A2-HS15464. When this switch is toggled to "OVER-RIDE", the
limit switches on the two tailgas valves are ignored by the
Complete Flowpath Interlock logic until the DCS operator
finishes routing the Train 1 SRU tailgas into the TGCU to
deactivate the over-ride. During this time, the DCS operator is
responsible for ensuring that there is always a complete
flowpath for the Train 1 SRU.
After the initial startup, the sulfur plants will contain some sulfur
throughout the system, and especially in the catalyst beds. Sulfur fires will
ignite at temperatures as low as 150°C if sufficient oxygen is available.
For this reason, it is very important to minimize the time periods when air
(or combustion gas containing oxygen) is routed through the catalyst
beds. Localized temperatures in excess of 150°C can exist in a catalyst
bed even though the temperatures measured around the Reactor are less
than 150°C. Because of this, sulfur ignition sometimes occurs in the
catalyst beds when it is not anticipated by temperatures that are readily
available for observation.
as it will require some time to cool down the hot spot before proceeding
with startup.
Do not use water to quickly cool a Reactor after a fire. Not only will this
damage the catalyst, the rapid cooling may cause structural damage to
the Reactor. The acidic water that forms may cause corrosion damage to
the Reactor or other equipment. Nitrogen is available in each SRU for use
in cooling a hot catalyst bed.
CAUTION
The combustion gases are routed to the atmosphere via the Thermal
Oxidizer. Therefore, normal operating procedures require that the
Thermal Oxidizer also be warming up according to its refractory warmup
schedule (or already be on-line) during the period when the SRU(s) is(are)
being brought up to operating temperatures. Do not admit acid gas to an
SRU until the Thermal Oxidizer is at operating temperature and ready to
accept SRU tailgas.
A. Open the Warmup Bypass Valves, and close the Tailgas Valve to the
Thermal Oxidizer and the Tailgas Valve to the TGCU. Startup
cannot be attempted unless this flow path is open.
B. Ignite the warmup burner in the Acid Gas Burner and fire on fuel gas
with excess air, adjusting air and fuel gas rates to follow the
appropriate warmup schedule.
C. Once the Waste Heat Boiler and Sulfur Condenser start to make
steam, their back-pressure controllers should be placed in service.
The other tube passes in the Sulfur Condenser and the tube passes
in the reactor feed heaters will come up to temperature as these
boilers begin producing steam.
D. When the furnace and all process heat exchangers are warmed up to
normal operating temperatures and the Thermal Oxidizer is ready to
accept SRU tailgas, reduce the fuel gas and air flow rates. Open the
Tailgas Valve to the Thermal Oxidizer, then close the Warmup
Bypass Valves. Add amine acid gas and reduce fuel gas in equal
increments until the fuel gas is shut off.
E. Gradually admit the full amine acid gas flow rate. Adjust the air flow
to the proper air:amine acid gas ratio. Follow the procedures in
these guidelines for introducing SWS gas into the SRU. Gradually
admit the full SWS gas flow rate and readjust the air:acid gas ratio if
necessary.
There are several advantages to using the cold bed startup procedure.
First, the catalyst beds are not exposed to warmup gases containing free
oxygen. This reduces the chance of fires in the catalyst bed during
warmup, which can cause overheating damage to both equipment and
catalyst.
Second, the catalyst beds are not exposed to warmup gases that contain
free carbon (soot). This reduces the chance of contaminating and
plugging the beds with soot.
Third, the cold bed startup procedure reduces catalyst sulfation and,
therefore, keeps the catalyst active longer. Deactivation has been shown
to be caused primarily by sulfate contamination of the catalyst surface.
Sulfation occurs most readily at conditions encountered during a startup
procedure which uses combusted fuel gas for catalyst heating.
All of the piping and valves in liquid sulfur service are steam-jacketed, as
are the valves in sulfur vapor service and the vent stacks on the Sulfur
Surge Tanks. The steam traps serving these heating systems should be
checked regularly to verify proper operation. The simplest method to do
this is to verify that sulfur will melt on the steam trap inlet; if the
condensate there is hot enough to melt sulfur, then the steam in the
jackets will be hot enough, too. It is also important to periodically sweep
the non-condensibles out of the jackets and coils by giving their vent
valves a good "blow". This will prevent the accumulation of
non-condensibles that could create localized "cold" spots where sulfur can
freeze.
CAUTION
Essentially all of the ammonia in the SWS gas will be destroyed in the
Reactor Furnace during normal operation. If, however, amine acid gas
flow is interrupted (due to upsets in the ARU, etc.) and the SRUs are
processing only SWS gas, the ammonia may not be completely destroyed
and salts could begin to form in the downstream equipment (particularly
the Sulfur Condensers). Loss of amine acid gas flow can also cause
excessively high furnace temperatures, poor sulfur recovery, and poor
operation or equipment damage in the TGCU or the Thermal Oxidizer
downstream. For this reason, the operator must closely observe the
SRUs if their amine acid gas flow is interrupted, and be ready to activate
the SRU ESD systems if necessary to prevent equipment damage.
The catalyst may also be fouled by passing fuel gas combustion products
through the beds when insufficient air to burn all of the fuel gas is being
supplied to the Acid Gas Burner. This causes soot (carbon) formation
which coats the catalyst and causes loss of activity. The catalyst beds in
this plant will be warmed with fuel gas combustion products only during
the initial startup. Excess air will be used during this warmup period, so
the chances of fouling the catalyst in this manner are remote.
The catalyst may also temporarily lose activity due to molten sulfur
condensing on the beds. This can be corrected by raising the Reactor
inlet temperatures by approximately 15-20°C for a few hours, then
readjusting to the normal operating range. The catalyst activity will be
completely restored in this manner by re-vaporizing the deposited sulfur.
The reactor feed temperatures can be raised by appropriate adjustment of
the temperature controllers on the gas outlet lines from the reheat
exchangers.
The acid gas flow controls for Train 1 SRU and Train 2 SRU are designed
to allow automatic operation of the parallel units in a fashion that
maximizes processing capacity and maximizes sulfur recovery efficiency.
There are two basic schemes for operating SRUs in parallel: "base-load"
operation of all-but-one SRU, or "cascade" operation of all SRUs. Each
scheme has advantages and disadvantages relative to the other,
depending on the operating characteristics of the particular feed units and
The overall sulfur recovery efficiency for the SRUs as a whole will depend
on how much acid gas is to be processed, the relative amounts of amine
acid gas and SWS gas to be processed, relative catalyst activities within
the reactors of the plants, and many other factors. As a result, the choice
of which operating mode to use will often depend on the particular
circumstances at any given time. As operating experience is gained with
the units, past experience will probably serve as the best tool for choosing
the operating mode in different situations.
The primary indication of blower surge is erratic air flow rate. The
first sign of this is usually audible – the check valve in the blower
discharge line begins to "clatter." The air pressure gauge on the inlet
to the Acid Gas Burner will usually fluctuate rapidly, and the burner
flame can often be observed to "puff" back and forth, when the
blower is in surge. If the surge is severe enough, it will cause high
vibration levels on the blower. If the blower is in surge for an
extended period, the blower casing will overheat due to re-circulation
of hot air between stages of the machine. Regardless of the
symptoms, the result of allowing a blower to operate in surge for long
periods of time is physical damage to the blower, either from high
vibration or from high temperature. For this reason, do not allow an
air blower to remain in surge.
To prevent the blower from surging at low flow rates, the discharge
piping on each blower has a "blow-off" valve installed. The action of
the blow-off valve is controlled by relays in the DCS. When the air
flow is low, the PLC will open the blow-off valve and allow some of
the air from the blower to vent to the atmosphere, increasing the air
flow through the blower to keep it above the surge line. A silencer
has been installed in the vent line to reduce the noise level around
the blower when the blow-off is used. If the blower is surging, then
adjust its blow-off valve to open more until the blower stops surging. It
does no harm to open the blow-off more than necessary, although it
does waste power by forcing the blower to compress more air than
necessary. Adjusting the amount that the blow-off opens is simply a
matter of making the appropriate configuration change in the DCS.
Since each SRU must remain on-ratio at all times for optimum sulfur
recovery, it is important that the air flow to an SRU not be disturbed
while swapping blowers. If the air flow fluctuates, the best that can
happen is a minor disturbance in air:acid gas ratio and a small drop
in sulfur recovery. At worst, the Acid Gas Burner may lose its flame,
the SRU will shut down on "flame failure", and the acid gases will be
diverted to the flare (a reportable emission episode). The "bias"
controllers in the DCS together with the bias and flow control relays
in the DCS, are designed to make swapping blowers relatively simple
and avoid these problems.
The bias relays in the DCS allow the DCS operator to slowly ramp up
the flow from the off-line blower while ramping down the flow from
the on-line blower. Although we have attempted to automate this
concurrent ramping operation on a couple of past projects, we have
not found this to be very satisfactory. The way that the blower
controls need to be ramped will depend on the current plant
throughput and whether or not the blower suction valve is still in
control of the air flow from the blower. This is classic "fuzzy logic",
something that is easy for a human to do but very difficult for a
computer.
The procedure below describes how to switch an SRU from the "A"
blower to the "B" blower. That is, the "A" blower is running to the
SRU and the "B" blower is not currently running. The procedure to
switch from the "B" blower to the "A" blower in the SRU is similar.
Make sure the SRU is operating stably before proceeding.
This means that its relay will be multiplying the signal it receives
from the process air flow controller by 0.0, so all of the flow
relays for the valves on the “B” blower will be receiving 0% as
their inputs. After transformation by the suction, discharge, and
vent relays in the DCS, this means that the positioners on the
suction valve, discharge valve, and vent valve will be receiving
control signals of 33%, 0%, and 100%, respectively.
This ensures that the input to the "bias" relays does not change
during the blower swap procedure, so that the DCS operator
can see the impact on air flow while adjusting the relays.
(2) Start the blower using its local start/stop control station.
The blower suction valve will open 33%, its vent valve will open,
and its discharge valve will remain closed. The valves will all
return to being closed if the blower is not started before the
"permit to start" times out.
Since the discharge valve will still be fully closed when the
blower starts, there will be no change in the air flow to the SRU
even though air will be flowing through the blower. All of the air
will be flowing out of the blow-off valve and venting atmosphere.
F. In the DCS, begin to increase the output from the “B” blower
hand controller.
This will begin to increase the multiplier in the “B” relay from
0.0, and the output to the discharge valve will begin to increase
as the output to the vent valve begins to decrease.
This will begin to reduce the multiplier in “A” relay from 1.0 and
begin to reduce the flow from the “A” blower. Depending on
current operating conditions in the SRU, this may be due to
throttling the suction valve more, or may be due to closing of
the discharge valve.
This will increase the air flow from the “B” blower and reduce
the air flow from the “A” blower until all the flow to the SRU is
from the “B” blower and the “A” blower is just venting air to the
atmosphere.
K. Shut down the “A” blower using the local start/stop control
station.
The amount of amine acid gas that is fed to the burner in the SRU is
controlled using the flow ratio controller in the DCS to adjust bypass gas
control valve to regulate the amine acid gas flowing to the side injection
ports on its furnace (the bypass gas flow rate). In theory, the optical
pyrometer mounted on the side of the furnace should measure the
temperature inside the first zone of the Reactor Furnace and make
appropriate adjustments to the bypass gas flow by changing the ratio
setting on the flow ratio controller to control the desired temperature.
0.215
0.214
0.213
0.212
Bypass Gas Ratio, Nm3/Nm3
0.211
0.209
0.208
0.207
0.206
0.205
0.00 0.01 0.02 0.03 0.04 0.05
The setpoint for the flow ratio controller can be set by the operator using
the graph above. When operating in this mode, the temperature indicated
on the optical pyrometer can be monitored to determine if changes to the
setpoint on the flow ratio controller are necessary. If the temperature
reading is lower than normal, raise the setpoint on the flow ratio controller
to bypass more amine acid gas around the burner and raise the
temperature. If the temperature reading is higher than normal, lower the
setpoint on the flow ratio controller to bypass less amine acid gas around
the burner and bring the temperature down.
Whether the bypass gas ratio is controlled directly or is set by the action of
the temperature controller adjusting the bypass gas ratio, the following
considerations apply to the bypass gas flow rate:
(7) The total bypass acid gas flow rate should never be allowed to
exceed 67% (i.e., ⅔) of the total amine acid gas flow rate, as this will
ensure that at least ⅓ of the total acid gas feed is always flowing to
the burner regardless of the SWS gas flow rate. If less that ⅓ of the
total H2S is fed to the burner, all of the oxygen in the process air fed
to the burner may not be consumed. If this happens, free oxygen
may enter the downstream catalyst beds and catch them on fire,
leading to catalyst (and possibly equipment) damage.
(8) 65% is the recommended maximum bypass acid gas ratio to allow a
safety margin for flow measurement errors, slow control response,
plant upsets, etc.
(10) The pressure drop through the Acid Gas Burner is the driving force
that allows the bypass gas control valve to bypass part of the amine
acid gas around the burner and into middle of the furnace instead.
When the SRU is operating at low flow rates, there may not be
enough pressure drop through the burner to give good control of the
bypass acid gas. In such cases, the flow ratio controller will "pinch"
the control valve in the acid gas line to the burner, increasing the
pressure drop available for the bypass gas control valve.
The DCS relay is designed to limit the output to the control valve in
the acid gas line to the burner so that this valve is never
completely closed. There should always be at least ⅓ of the amine
acid gas flowing to the burner to be sure that the front zone of the
Reactor Furnace does not begin to operate in an oxidizing
atmosphere.
WARNING
Surprisingly, though, we have found that our clients do not always operate
our SRUs in strict accordance with the published operating procedures
regarding such matters as minimum furnace temperature, feedstock
ratios, etc. In fact, some of our clients have operated their SRUs on just
sour water stripper off-gas for days at a time because of operating
problems in the amine unit. Although there was undoubtedly ammonia
escaping from the furnace when operated in this manner, there has never
been any plugging with salts during this time.
This has led us to conclude that avoiding SO3 formation, not complete
ammonia destruction, is the critical element in the reliability of our
reducing-mode SRUs. If you examine the melting points of the various
salts that can result from ammonia and the sulfur compounds that might
be found in a sulfur plant, only ammonium sulfate, (NH4)2SO4, has a
melting point that is higher than the freezing point of sulfur. Since all of
the surfaces in a sulfur plant must be maintained above the sulfur freezing
point, none of the other salts can precipitate under normal operating
temperatures. Thus, as long as the furnace is operated in a reducing
atmosphere so that there is no SO3 to combine with water and the
The air demand analyzer will continuously analyze the process gas
and calculate the percent air demand, allowing the air demand
controller to automatically trim the air:acid gas ratio to stay close to a
2:1 H2S:SO2 ratio. If the analyzer is out of service or needs to be
checked, the procedures in Section 9.10 of these guidelines can be
used to manually sample the process gas and determine the
H2S:SO2 ratio, so that the appropriate change can be made to the
air:acid gas ratio.
However, lowering the feed temperature to the first catalyst bed may
not increase recovery, due to lower hydrolysis of organic sulfur
compounds in this catalyst bed. Calculations indicate that the
optimum sulfur recovery for these SRUs is obtained then the first
catalyst bed is operated at high temperature, due to the higher
conversion of the organic sulfur compounds to H2S, which is
subsequently recovered in the downstream catalyst beds. As shown
on the Process Flow Diagram, the feed temperature to the first
catalyst bed will normally be around 225-235°C. Operating
experience will show whether lower reactor outlet temperatures still
(4) If the SRU must operate at low flow rates permanently, or for
long periods of time, installing new orifice plates with smaller
bores may be an attractive solution. This will increase the
differential pressures measured by the meters to put the flow
transmitters back into good operating ranges. The
disadvantages of this technique are that a plant shutdown is
required to make the change, and that the plant cannot operate
at high flow rates again without changing orifice plates.
(6) If the SRU must operate at variable flow rates, using dual flow
transmitters calibrated for low and high differentials can provide
accurate flow measurement over a much wider range. With
proper programming in the DCS, the dual transmitters allow
"seamless" metering of the flow.
The feed heaters cannot vaporize all of the carry-over liquid sulfur,
probably because the small surface area of the droplets (relative to
their volume) causes slow mass transfer of vaporized sulfur away
from the droplets that impedes heat transfer. This causes the liquid
sulfur droplets to enter the reactor catalyst beds. The liquid sulfur is
then adsorbed into the pores of the catalyst where it blocks the active
sites, rendering the catalyst inactive. The catalyst activity can be
restored by raising the reactor feed temperature and vaporizing the
liquid sulfur out of the pores, but this can be very hard to do when the
condensers are carrying over liquid sulfur.
Experience has shown that when the condenser passes begin to fog,
the liquid sulfur will accumulate in the outlet channels of the heating
passes in this style of sulfur plant. Due to the arrangement of these
"package" sulfur plants, the heating pass outlet channels are low
spots in the flow paths from the condenser outlets to the reactor
inlets. It is believed that as the gas flowing out of the heating pass
tubes turns 90° to exit through the channel outlet nozzles, centrifugal
force causes the sulfur droplets to impinge upon the endplates of the
channels with enough force to make the small droplets coalesce into
droplets too large to leave with the gas. Over a period of time, sulfur
will accumulate to the point where it begins to cause fluctuations in
the operating pressure of the affected SRU. The pressure drop will
build up enough to "lift" some of the sulfur into the downstream
catalyst bed, at which point the pressure drop will immediately
become much lower.
operation of the downstream catalyst beds if the drain valves are left
open.
To make firing supplemental fuel gas easier, the air flow control
system is designed to automatically add air for the fuel gas like it does
for the acid gas. The air:acid gas ratio control system will
automatically add more process air for the fuel gas when firing
supplemental fuel gas. The air demand analyzer in the SRU will
continue to keep the air flow at the proper rate via the air controller.
tubes so that they are then above the "fog" formation rate and sulfur
carry-over is eliminated. Soft iron plugs can be inserted into the inlet
ends of the tubes for this purpose. (Do not plug the outlet ends of
the tubes. Since the boiler slopes from its inlet end to its outlet end,
liquid sulfur would accumulate in the tubes and could cause localized
corrosion, plugging, etc.)
The first step in identifying the cause of the high pressure drop is to
determine which equipment pass or section of piping contains the
restriction. (It is unusual to have more than one area of high pressure
drop at any one time.) This is best accomplished by making a pressure
survey of the process side of the SRU (and Tailgas Cleanup Unit and
Thermal Oxidizer, if necessary).
Beginning at the front end of the sulfur plant of interest, use the pressure
tap valves on the inlet and outlet lines from each equipment pass to
measure the pressure at each point in the process. Proceed toward the
back end of the process until the pass with the high pressure drop is
found. Note that some of the pressure tap valves may be plugged with
solid sulfur. Rod-out the sample valves as necessary to obtain an
accurate pressure reading.
WARNING
There are many qualified boiler and water treatment companies that can
advise the owner/operator on chemical treatment testing and controls. It
is recommended that only those companies that have local technicians
with extensive experience specifically in boiler water treatment be
selected to assist with Samsung Total Petrochemicals Co., Ltd.’s program.
The design details incorporated in the boilers in these SRUs have proven
to be very reliable when combined with good operator practice regarding
water treatment. However, even properly designed equipment can be
severely damaged during a short period of operation if the water treatment
program is inadequate or improper.
The Waste Heat Boilers and the Sulfur Condensers are equipped with
continuous blowdowns to remove suspended and dissolved solids from
the water inside the boilers. In addition, these boilers are equipped with
intermittent blowdown connections on the bottom of their shells. These
intermittent blowdown valves should be used on a regular basis to give
the boilers a good "blow" to prevent sludge from accumulating in the
bottom of the shells. This is particularly important for the Waste Heat
Boiler because sludge must not be allowed to coat the tubes. The
consequence of fouling the outside of the tubes is tube failure from
overheating, as the fouling will impair the heat transfer and allow the hot
combustion gases to destroy the tubes.
Prior to using the intermittent blowdown valves, use the level controllers in
the DCS to raise the water level up to the high level alarm point. Then
open the intermittent blowdown valves, one at a time, until the level drops
back to the normal liquid level. Watch the boiler level in the sight glasses
throughout this operation to ensure that the level is not lost (which would
activate the SRU ESD and shut down that plant). Remember to reset the
level controllers at the conclusion of this procedure.
C. Check the rotation of the Process Air Blowers, the Acid Gas
Knock-Out Drum Pumps, and the SWS Gas Knock-Out Drum
Pumps:
(2) "Bump" each Acid Gas Knock-Out Drum Pump and check for
proper rotation.
(3) "Bump" each SWS Gas Knock-Out Drum Pump and check for
proper rotation.
D. Check all piping and equipment to be sure that all blinds have been
removed and that no valves are vented to atmosphere.
I. Fill the boilers with treated boiler feed water back up to the normal
liquid levels.
L. Check all relief valves to ensure that they are installed in the proper
locations and set for the correct relieving pressures.
CAUTION
The process piping and equipment in each SRU can be checked for leaks
by using a Process Air Blower to pressurize the process side of the
equipment and piping to about 0.6-0.7 kg/cm2(g), then checking flanges,
etc. for leaks (usually by applying masking tape or "Snoop" to the flanges,
and by listening for other leaks). In order to develop this pressure, the
blower can be operated with the tailgas block valves and the warmup
bypass valves in the SRU closed, and the blow-off valve on the blower
"pinched". This procedure requires some special preparations to operate
the blower in this manner, as detailed below.
This same procedure can be used to leak test each SRU before restarting
it following maintenance. Whenever plant maintenance requires opening
one or more of the flanged connections in an SRU, it is good practice to
leak test that SRU before returning it to service. This allows detecting any
Note that the SRU warmup bypass line is not leak tested during this
procedure. This line can be checked for leaks using the nitrogen purge on
the piping as described in a later section of these guidelines.
M. Switch the process air flow hand switch in the DCS to "local" to give
control of the valves on the air blower to the air flow controller (HIC)
on the local SRU control panel.
N. Confirm that the Reactor Cool-Down switch on the local SRU control
panel is set to "NORMAL".
O. Confirm that the manual block valve in the SRU Tailgas line is open.
(2) The nitrogen purge valve between the warmup bypass valves is
closed.
Confirm that the "WARMUP OPEN" light on the panel is illuminated, and
that the "TTO OPEN" and the "TGCU OPEN" lights on the panel are
extinguished.
Q. Turn the Leak Test key switch on the local SRU control panel to
"TEST".
(3) All of the ESDs for that SRU are bypassed, except for the
high-high furnace pressure S/D and the manual S/D switches.
Confirm that the "WARMUP OPEN" light on the local SRU control panel
is now extinguished.
R. Set the air flow controller on the local SRU control panel to 0%
output and confirm that the suction, discharge, and blow-off valves
on the air blowers are fully closed.
(1) Press the local "permit to start" push-button for the selected
blower.
(2) Start the blower using its local start/stop control station.
The blower suction valve will open 33%, its vent valve will open, and
its discharge valve will remain closed when the "permit to start"
push-button is pressed. Once the blower is started and comes up to
speed, a flow of air will be established out of the blow-off valve and
its silencer.
T. Use the local air flow controller as needed to open the discharge
valve on the blower and send air to the SRU to begin pressurizing it.
Although the blower discharge valve will begin to open as the output
from the controller is increased, air will not flow through the sulfur
plant once pressure builds because the warmup bypass valves and
the tailgas valves are all closed.
At this point, two operators will be necessary to control and monitor the
Process Air Blower. One operator should be stationed at the local SRU
control panel, and one stationed near the blower area.
CAUTION
U. Slowly increase the output from air flow controller to "pinch" the
blow-off valve on the air blower until the discharge pressure from the
blower reaches 0.6-0.7 kg/cm2(g) as measured by the pressure
gauge on the process air line to the burner.
Due to the volume inside the SRU, it will take several minutes for the
pressure to build up in the SRU.
V. Once the desired discharge pressure has been achieved, and the
blower is operating stably, check all of the equipment and piping
connections for visible or audible signs of leakage. Continue to
monitor the air blower to be sure it is operating stably.
W. After the leak test has been completed, press the ESD push-button
on the local SRU control panel to activate the SRU ESD system and
shut down the air blower.
X. Turn the Leak Test switch on the local SRU control panel to
"NORMAL".
(3) All of the ESDs for the SRU are enabled again.
Confirm that the "WARMUP OPEN" light on the local SRU control panel
is now illuminated.
(1) The air blower is shut down, and its suction, discharge, and
blow-off valves are closed.
(3) The Tailgas Valve to the Thermal Oxidizer and the Tailgas
Valve to the TGCU are both closed.
WARNING
A. Verify that the blinds are in place in the inlet amine acid gas line and
the inlet SWS gas line. Do not attempt this procedure if these lines
are not blinded from their respective acid gas sources.
C. Open the suction valve and close the discharge valve on each Acid
Gas Knock-Out Drum Pump.
D. Open all of the vent and drain valves on the level and pressure
instruments on the Acid Gas Knock-Out Drum and each Acid Gas
Knock-Out Drum Pump, and the vent and drain valves on each Acid
Gas Knock-Out Drum Pump.
E. Remove the blind from the drain valve on the pump suction line and
use a hose or other means to temporarily connect nitrogen to the
valve. Commence the flow of nitrogen into the Acid Gas Knock-Out
Drum and each Acid Gas Knock-Out Drum Pump, so that nitrogen is
flowing out of all of the open valves. Be sure to include the acid gas
inlet line from the Amine Regeneration Unit.
G. When the oxygen concentration is below 1%, begin closing the vent
and drain valves. Close the valves on each Acid Gas Knock-Out
Drum Pump first, then the valves on the Acid Gas Knock-Out Drum
level instruments. Leave the sample connection valve open on the
outlet line from the Acid Gas Knock-Out Drum.
H. Close the valve where the nitrogen hose is connected to stop the
flow of nitrogen, then close the sample connection valve.
I. Repeat Steps C through H for the SWS Gas Knock-Out Drum and
the SWS Gas Knock-Out Drum Pump. The sample connection valve
on the outlet line from the SWS Knock-Out Drum should be the last
valve closed, after stopping the flow of nitrogen.
Leave each system blocked-in like this until ready to bring acid gas into
the SRU.
A. Select local manual control for the main fuel gas control valve by
switching the fuel gas hand switch in the DCS to "local".
B. Set the fuel gas controller on the local SRU control panel to 0%
output.
C. Confirm that the following fuel gas and instrument air valves are
closed:
(7) The manual block valve in the main fuel gas supply line.
(8) The two automated block valves and the flow control valve
downstream of the manual block valve in the main fuel gas line
to the Acid Gas Burner.
(9) The upstream manual block valve, the two automated block
valves, and the downstream manual block valve in the fuel gas
supply line to the pilot.
(10) The manual block valve(s), and the automated block valve in
the air supply line to the pilot.
(11) The manual block valve in the instrument air supply line to the
Air Demand Analyzer.
(12) The block valves in the instrument air supplies to the level
transmitters, on the Sulfur Surge Tank.
D. Confirm that all of the manual vent/drain valves in the main fuel gas,
pilot fuel gas, and pilot air piping are closed.
E. If the orifice plate has already been installed in the fuel gas flow
meter remove it for now.
F. Disconnect the fuel gas and instrument air from the burner systems
by performing the following steps:
(1) Unbolt the flanged connection at the burner in the main fuel gas
supply line.
(2) Disconnect the fuel gas supply tubing where it connects to the
pilot.
(4) Cover the open ends of these connections on the burner and
pilot to prevent debris from entering when the upstream piping
is blown down.
(1) The automated block valves in the main fuel gas supply line.
(2) The automated block valves in the fuel gas supply line to the
pilot.
(3) The automated block valve in the instrument air supply line to
the pilot.
J. "Crack" the manual block valve in the main fuel gas supply line and
allow fuel gas to blow through the piping until it is clear. Then close
the gate valve, reinstall the main fuel gas pressure regulator, and
reopen the block valve.
K. Using the pressure gauge and the vent valve downstream of the
main fuel gas pressure regulator, adjust the main fuel gas regulator
to its specified setpoint.
L. Use the main fuel gas flow controller on the local control panel to
fully open the fuel gas flow control valve in the main fuel gas line,
then use the downstream vent valve to blow out this section of
piping. Close the vent valve when the piping is clear.
M. "Crack" the manual block valve downstream of the fuel gas flow
control valve and allow fuel gas to blow through the piping until it is
clear. Then close the manual block valve and the control valve.
N. "Crack" the upstream manual block valve in the fuel gas supply line
to the pilot and allow fuel gas to blow through the piping until it is
clear. Then close the ball valve, reinstall the pilot fuel gas pressure
regulator and reopen the block valve.
O. Using the pressure gauge and the vent valve downstream of the pilot
fuel gas pressure regulator, adjust the pilot fuel gas regulator to its
specified setpoint.
Q. "Crack" the upstream manual block valve in the instrument air supply
line to blow air through the piping until it is clear. Then close the
block valve, reinstall pressure regulator the instrument air pressure
regulator and reopen the block valves.
R. Using the pressure gauge and the vent valve downstream of the
instrument air pressure regulator, adjust the pilot instrument air
regulator to its specified setpoint.
T. Disconnect the air supply line at the Air Demand Analyzer, cover the
open end of the downstream piping, and "crack" the manual block
valve to blow air through the piping until it is clear. Then close the
manual block valve, reconnect the piping, and reopen the block
valve.
cover the opening. Open the block valve briefly to blow any liquids
or debris from the purge line, then reconnect the purge to the bubbler
tube. Reopen the block valve and adjust the FI to a small air flow
(0.8-1.6 Nm3/Hr). Place the other level transmitters in service in the
same manner.
V. Remove the "forces" from the PLC and confirm that all of the
automated block valves close and all of the automated vent valves
open.
W. Close the manual block valve in the main fuel gas supply line and the
manual block valve in the instrument air line supply until the SRU is
ready for startup.
X. Reconnect the fuel gas and instrument air to the burner systems by
performing the following steps:
(1) Bolt the flanged connection at the burner in the main fuel gas
supply line back together.
(2) Reinstall the fuel gas supply tubing where it connects to the
pilot.
(4) Reinstall the orifice plate in the fuel gas flow meter.
(1) The manual block valves in the N2 purge line to the bypass acid
gas injection nozzles on the Reactor Furnace.
(2) The ball valves in the purge lines to the burner instruments.
(3) The block valves in the purge lines to the optical pyrometer.
(4) The gate valves in the nitrogen supply lines located near the
Reactor and the nitrogen supply line located near the Acid Gas
Burner.
(5) The ball valves in the purge lines to the SWS gas flow
transmitter and pressure gauge.
(6) The gate valve in the nitrogen supply line to the Air Demand
Analyzer.
(7) The gate valve upstream and the ball valve downstream of the
rotometer in the purge line on the SRU warmup bypass line.
B. Confirm that the H.P. nitrogen and L.P. nitrogen supply headers have
been placed in service, with the pressure regulator(s) set at the
values specified on the P&IDs and safety relief valves in service, and
that the main supply header piping has been blown down and
drained.
C. Open the gate valve in each of the three nitrogen supply lines
located near the Reactor and the nitrogen supply line near the Acid
Gas Burner until each line is clear.
D. Remove pressure regulator in the purge line for the optical pyrometer
viewport and nozzle, cover the open end of the downstream piping,
open the gate valve, and "crack" the ball valve in the supply line to
blow nitrogen through the piping until it is clear. Then close the gate
valve and the ball valve and reinstall the regulator.
F. Open the gate valve and the ball valve in the nitrogen supply. Using
the pressure gauge, adjust the regulator to its specified setpoint.
Allow nitrogen to blow through the tubing until it is clear. Reinstall
the purge tubing to the pyrometer. Leave the gate valve and the ball
valve in the supply line open.
G. Remove the plug and use the drain valve at the end of the supply
line to the purges for the burner instruments to blow out this section
of piping until it is clear, then close the drain valve and reinstall the
plug.
H. Each of the low pressure purges for the burner instruments and for
the bypass acid gas nozzles has a rotameter (FI) near where it
connects to the process. Disconnect the upstream fitting at each FI
and cover the opening, then open its upstream ball valve briefly to
blow any liquids or debris from the purge line. Reconnect each FI,
disconnect the fitting where each purge enters the process and cover
the opening, open its upstream ball valve, then open its downstream
valve briefly to blow any liquids or debris from the purge line. Then
reconnect each purge to the process and open its downstream valve
to place it in service.
I. The SWS gas flow transmitter has low pressure purges for both of its
sensing lines, each with a rotameter near where it connects to the
sensing line. Disconnect the upstream fitting at each FI and cover
the opening, then open its upstream ball valve briefly to blow any
liquids or debris from the purge line. Reconnect each FI, disconnect
the fitting where each purge connects to the sensing line and cover
the opening, open its upstream ball valve, then open its downstream
ball valve briefly to blow any liquids or debris from the purge line.
Then reconnect each purge to the sensing line and open its
downstream ball valve to place it in service.
NOTE: The two rotameters must be adjusted to the same flow rate
so that the pressure drop of the purge gas in the sensing
lines does not affect the reading of the flow transmitter.
One way to do this is to confirm that the equalizing valve on
the flow transmitter manifold is closed, set the rotameter on
the upstream sensing line to a small flow rate
(~0.8-1.6 Nm3/Hr), and then adjust the flow rate of the other
rotameter until the flow meter reads zero.
J. The SWS gas pressure gauge also has a low pressure purge for its
sensing line with a rotameter near where it connects to the sensing
line. Disconnect the upstream fitting at the FI and cover the opening,
then open its upstream ball valve briefly to blow any liquids or debris
from the purge line. Reconnect the FI, disconnect the fitting where
the purge connects to the sensing line and cover the opening, open
its upstream ball valve, then open its downstream ball valve briefly to
blow any liquids or debris from the purge line. Then reconnect the
purge to the sensing line and open its downstream ball valve to place
it in service.
M. Open the manual block valve downstream of the FI and allow the
nitrogen to pressurize the piping between the two Warmup Bypass
Valves. Check all of the piping connections for visible or audible
signs of leakage (by applying masking tape or "Snoop" to the
flanges, listening for other leaks, etc.). When this leak checking
complete, if the PLC was "forced" in the previous step, remove the
"force" and confirm that the Warmup Bypass Valves open and the
purge valve closes. Leave the manual block valve downstream of
the FI open.
A. Confirm that the steam supply valves to the steam coils in the Sulfur
Surge Tank are all closed, and that the steam trap stations on each
of the coils are all blocked in.
C. Establish steam flow into each of the coils by opening the steam
supply valves to each coil.
D. Allow air (and any liquids or debris) to purge from the vent valves.
Close each vent valve as it begins to blow steam.
E. Open the upstream block valve of the steam trap on each coil and
use the bleeder on each trap to drain water (and any other liquids)
from each coil. Close the bleeder on each trap once hot condensate
begins flowing through the trap.
F. Open the test valve on each trap and confirm that each trap is
operating properly. Then close the test valve and open the
downstream block valve on each trap to place the traps in service to
the condensate header.
I. Make sure that the breather vents at each end of the Sulfur Surge
Tank are unobstructed and that the air sweep vent stack has begun
to draft air into the tank through the breather vents.
J. Check that the suction valve on the Sulfur Surge Tank Vent Ejector is
closed and the discharge valve is open.
K. Confirm that the globe valve in the motive steam line to the Sulfur
Surge Tank Vent Ejector is closed, then open the upstream manual
block valve in the line.
L. Slowly open the globe valve to establish motive steam flow to the
ejector. Verify that the steam is flowing at the proper rate (about
500 kg/H) on the steam flow meter in the DCS.
M. Open the ejector suction valve. The ejector should now begin to
overcome the natural-draft driving force of the air sweep vent and
route the ventilation air from the pit to the Thermal Oxidizer.
N. Confirm that all steam traps are functioning properly and that steam
is flowing to the ejector before directing your attention away from the
Sulfur Surge Tank.
Pre-filling of the seals can be accomplished at any time after the steam
heating for the sulfur rundown lines and Drain Seal Assemblies has been
placed in service as described in the preceding section. Both molten
sulfur and solid sulfur prills have been used for this purpose. If sulfur prills
are used, proceed slowly enough so that the steam jackets on the seals
can melt the sulfur. Continue to add sulfur to each seal until molten sulfur
pours from its spill-over spout into its collection basin. Then bolt the blind
flange back on the top of each seal assembly.
If the drain seals are pre-filled in this fashion, the block valves in the sulfur
rundown lines can be left open during the initial plant startup. Otherwise,
these block valves must be closed when acid gas is first introduced to
prevent hazardous process gases from escaping from the SRU.
Section 9.8.2 of this manual describes how to use the sulfur produced
during startup to fill the drain seals if they are not pre-filled.
During the initial startup, the Reactor Furnace and downstream equipment
will be warmed up to operating conditions following the refractory vendor's
cure-out schedule for the Reactor Furnace.
CAUTION
B. Confirm that the manual block valve in the SRU tailgas line is
open.
C. Confirm that the amine acid gas flow on/off switch, is set to "on"
so that this flow will be included in the air:acid gas ratio control
system.
F. Place the air demand controller in "manual" and set its output to
50%.
G. Confirm that the manual signal bias control for the blower to be
used is set to 100% so that the control signals to the blower
valves are not modified.
H. Select local manual control for the fuel gas flow control valve,
by switching the main fuel gas hand switch (HS) in the DCS to
"local".
J. Confirm that the fuel gas flow on/off switch is set to "on" so that
this flow will be included in the air:acid gas ratio control system.
L. Place the bypass acid gas flow ratio controller in "manual" and
set its output to 0% so that control valve the bypass acid gas
control valve will be fully closed.
N. Verify that the four block valves in the sulfur rundown lines from
the Sulfur Condenser are closed (unless the Sulfur Drain Seal
Assemblies have been pre-filled with sulfur as described in
Section 9.7.8 of this manual).
Loosen the wing nut on the hinged pyrometer fixture and swing
the pyrometer out of the way. Unscrew the viewport len and
remove it (be careful with the rubber o-ring gasket). Store the
viewport lens in a safe place. Screw the thermocouple adapter
housing onto the pyrometer mounting plate (with the o-ring in
place). Open the pyrometer block valve, slide the thermocouple
into the furnace, and tighten the packing gland on the end of the
adapter housing.
P. Confirm that the Acid Gas Firing switch on the local SRU
control panel is set to "DISABLED".
Q. Confirm that the Leak Test switch on the local SRU control
panel is set to "NORMAL".
S. Set the manual amine acid gas control (HIC) on the local SRU
control panel to 0% output.
Visually confirm that the amine acid gas inlet valve is closed.
T. Set the manual SWS gas control (HIC) on the local SRU control
panel to 0% output.
U. Set the manual fuel gas control (HIC) on the local SRU control
panel to 0% output.
Visually confirm that the main fuel gas valve and the two
automated shutdown valves are closed.
V. Set the manual air control on the local SRU control panel to 0%
output.
W. Verify that the acid gas control valve in the amine acid gas line
to the burner is fully open.
X. Verify that the bypass acid gas control valve in the bypass acid
gas line is fully closed.
Y. Verify that the pilot burner mounting nozzle is being purged with
nitrogen as indicated by its rotameter.
The "TTO OPEN" status light will flash until this valve has
moved to the proper position, then will be extinguished.
The " TGCU OPEN" status light will flash until this valve has
moved to the proper position, then will be extinguished.
B. Verify that the local start/stop controls for the Process Air
Blowers have their selector switches turned to the "STOP"
position.
(2) Start the blower using the local start/stop control station for
that blower.
E. Confirm that the air blower is running, then press the "ESD
RESET" push-buttonon the local SRU control panel to reset the
SRU ESD and extinguish the "RESET REQUIRED" light. This will
illuminate the "PURGE REQUIRED" light.
For safety reasons, the PLC will not allow the light-off
sequence to proceed until all these conditions are
satisfied. Once the problem with the valves, their
limit switches, or the pressure transmitters has been
corrected, the "LIMITS SATISFIED" light will stop
flashing and glow steadily, and the light-off sequence
can proceed.
G. Adjust the output of the air flow control (HIC) on the local SRU
panel to open the blower control valves and allow a large air
flow, 80% or more on the flow indicator on the local SRU control
panel, to purge the entire system for about 5 minutes. The
"PURGE REQUIRED" light will be extinguished and the "PURGE
COMPLETE" light will be illuminated after about 30 seconds, but
continue to purge the system for a full 5 minutes prior to this
first time ignition attempt.
(1) The manual block valve(s) in the main fuel gas supply line.
(2) The manual block valve(s) in the fuel gas supply line to the
burner.
(3) The manual block valve(s) in the fuel gas supply to the
pilot.
I. Adjust the output of the air flow control (HIC) on the local SRU
panel to reduce the air flow to 10-20%. This will extinguish the
"PURGE COMPLETE" light and illuminate the "PERMIT TO IGNITE"
light and the PLC will "enable" the ignition circuit.
(1) The nitrogen purge valve for the pilot burner is closed.
(3) The pilot gas automated vent valve is closed and the
automated block valves are opened.
K. The air and fuel gas pressure regulators for the pilot may
require some adjustment when first put in service before the
pilot will light. However, once set properly, the pilot should
ignite readily on subsequent startups. Refer to Section 9.11 of
these guidelines for a suggested procedure to adjust these
regulators.
(4) The startup bypass in the PLC for the "flame failure" S/D is
disabled.
N. After the pilot is lit, use the air flow control (HIC) on the local
SRU panel to increase the air flow rate to about 50% of scale,
or as high a rate as can be maintained without blowing the pilot
out. When curing refractory, it is best to keep the air flow as
high as possible to help distribute the heat more evenly and to
heat the downstream equipment more quickly.
The "TTO OPEN" status light will flash until this valve has
moved to the proper position, then remain steadily
illuminated.
(2) After the limit switches prove this valve open, the two
Warmup Bypass Valves are closed.
The "WARMUP OPEN" status light will flash until these valves
have moved to the proper position, then will be
extinguished.
(3) After the limit switches prove that at least one of these
valves is closed, the nitrogen purge valve to the Warmup
Bypass Line is opened.
B. Open the vent valves on each of the two boilers to vent air from
the steam sections.
C. Confirm that the BFW level controllers and control valves to the
Waste Heat Boiler and Sulfur Condenser are in service and
functioning properly.
D. The heat input from the pilot should be sufficient to reach the
first "hold" point in the refractory warmup schedule, 100-150°C.
If the temperature is too high, increase the air flow rate. If the
temperature is too low, decrease the air flow rate.
A. Confirm that the flow control valve in the main fuel gas line is
fully closed.
B. Confirm that the manual block valve(s) in the main fuel gas line
to the burner is (are) open.
C. If the air flow rate is not at 50% of scale, use the air flow control
(HIC) on the local SRU panel to set the air flow at about 50% of
scale.
(1) The nitrogen purge valve for the main warmup burner is
closed.
(3) The main fuel gas automated block valves are opened.
(4) The "MAIN FUEL ON" light on the local control panel is
illuminated.
E. Adjust the output of the main fuel gas flow control (HIC) on the
local SRU control panel to slowly open the control valve to
commence fuel gas flow to the warmup burner ring. Adjust the
Note that the fuel gas flow rate will be indicated on the local
panel and in the DCS.
A. Adjust the fuel gas flow rate with the main fuel gas flow control
(HIC) on the local control panel as necessary to cause the
furnace temperature to follow the refractory cure-out schedule
for the initial cure supplied by the refractory vendor.
It is often helpful to maintain a log of the air flow, the fuel gas
flow, and the furnace temperature during the cure-out for future
reference.
F. Once the third "hold" point in the cure-out schedule has been
reached (about 500°C), the optical pyrometer can be placed in
service. After the furnace temperature has stabilized, loosen
the packing gland on the thermocouple adapter housing and
slide the thermocouple out until the "keeper" stops it. Close the
pyrometer block valve then unscrew the adapter housing and
(1) The feed temperatures to all three chambers of the Reactor are
205°C or higher.
(4) All vent and drain valves on the Acid Gas Knock-Out Drum, its
piping, and the Acid Gas Knock-Out Drum Pump are closed
and plugged.
(5) Any blinds installed in the amine acid gas line have been
removed.
(6) The block valves are lined up to place an Acid Gas Knock-Out
Drum Pump in service, the selector switch on that pump is set
to "AUTO", and the pump level control transmitter is in service.
B. Confirm that the bypass acid gas flow ratio controller in the DCS is
still in "manual" with its output set to 0%. This ensures that the
bypass acid gas control valve will remain closed so that all of the
amine acid gas will flow to the Acid Gas Burner.
C. Adjust the process air flow rate to 50% of scale on the local indicator
using the air flow control (HIC) on the local SRU panel. Reduce the
fuel gas flow rate to 50% of scale on the local indicator using the
main fuel gas flow control (HIC) on the local panel.
D. Because of the procedure used for this initial firing, the Warmup
Bypass Valves are already closed and the Tailgas Valve to the
Thermal Oxidizer is already opened. Thus, the flowpath through the
SRU is already set correctly for introducing acid gas.
E. Switch the Acid Gas Firing selector switch on the local SRU control
panel to "ENABLED".
F. Slowly increase the output from the amine acid gas flow control (HIC)
on the local SRU control panel to begin opening the amine acid gas
inlet valve until the acid gas flow rate is approximately 10% on the
indicator on the local SRU control panel.
G. As soon as the acid gas flow rate reaches 10%, use the main fuel
gas flow control (HIC) to reduce the fuel gas flow rate from 50% to
40% on the local indicator.
H. Continue to add amine acid gas in 10% increments and reduce the
fuel gas in 10% increments until the fuel gas control valve is
completely closed.
I. Press the “FUEL GAS OFF” push-button on the local SRU control panel.
The PLC performs the following actions to "double block and bleed"
the main fuel gas:
(1) The main fuel gas automated block valves are closed.
(3) The nitrogen purge valve for the main burner is opened.
Verify that the that the fuel gas valves have moved to their proper
positions and that the main fuel gas burner ring is being purged with
nitrogen as indicated by the associated rotometer.
J. Press the "PILOT OFF" push-button on the local SRU control panel.
The PLC performs the following actions to block the pilot air and
"double block and bleed" the pilot fuel gas:
(1) The aitmated block valve in the air supply to the pilot is closed.
(2) The pilot fuel gas automated block valves are closed.
(4) The automated nitrogen purge valve for the pilot burner is
opened.
Verify that the air and fuel gas valves have moved to their proper
positions and that the pilot burner is being purged with nitrogen as
indicated by the associated rotameter.
K. Continue to slowly increase the output from the amine acid gas flow
control (HIC) to 100% so that the amine acid gas inlet valve is fully
open.
L. If the amine acid gas flow rate (in percent) displayed on the local
control panel is significantly different from the air flow rate (in
percent) displayed on the local control panel, use the air flow control
(HIC) on the local SRU panel to adjust the air flow until the
percentages are about the same. This should put the air:acid gas
ratio reasonably close to where it should be.
(1) The two manual block valve(s) in the main fuel gas line.
(2) The manual block valve(s) in the fuel gas to the pilot.
(3) The manual block valve(s) in the instrument air to the pilot.
N. Loosen the packing gland on the pilot and retract or extract the pilot
assembly:
(c) Verify that the pilot burner is still being purged with
nitrogen as indicated by the associated rotameter.
(b) Close the block valve to isolate the pilot from the furnace.
(c) Close the block valve in the nitrogen purge to the pilot
burner.
(d) Disconnect the chain and remove the pilot assembly and
store it in a safe place.
(3) Verify that the pilot burner mounting nozzle is still being purged
with nitrogen as indicated by the associated rotometer.
(1) Confirm that the air demand controller in the DCS is in "manual"
and its output is set at 50%.
(2) Confirm that the process air flow controller in the DCS is in
"cascade".
(3) Confirm that the output of the process air flow controller is
tracking the output of the manual air control on the local SRU
control panel.
(4) Confirm that the setpoint of the process air flow controller is
tracking its current reading.
(5) Confirm that the "coarse" setting of the air:acid gas manual ratio
set (HIC) is being back-calculated so that the remote setpoint it
supplies to the process air flow controller matches the current
"local" air flow setpoint on the controller.
(6) Switch the process air hand switch (HS) from "local" to
"remote".
The DCS process air flow controller now has control of the control
valves on the Process Air Blower, so that the process air flow rate
will be ratio-controlled automatically with the amine acid gas flow
rate. The output from the manual ratio set (HIC) will remain fixed at
its last value.
properly.
Q. If the Sulfur Drain Seals were not pre-filled with liquid sulfur to seal
them prior to startup, the block valves in the rundown lines will all be
closed at this time. After operating on acid gas for about 30 minutes,
open the block valve on the first condenser pass drain line.
Sufficient sulfur should have been produced by then to seal this drain
seal. If the drain seal does not seal within 30 seconds, close the
valve and try it again every 30 minutes or so until it seals.
R. After the first drain seals, open the block valve to the second drain
seal at approximately one hour intervals until it seals. Repeat this
with the third and fourth drain seals.
WARNING
(1) Confirm that the Waste Heat Boiler steam pressure controller is
set at 48.5 kg/cm2(g) and is controlling.
If the H2S:SO2 ratio is higher than 2:1, the SRU is running with less
than optimum air (i.e., "air deficient"). Increase the setting on the
air:acid gas manual ratio set (HIC) to raise the air:acid gas ratio and
reduce the H2S:SO2 ratio in the process gas.
If the H2S:SO2 ratio is lower than 2:1, the SRU is running with more
than optimum air (i.e., "excess air"). Reduce the setting on the
air:acid gas manual ratio set (HIC) to lower the air:acid gas ratio and
increase the H2S:SO2 ratio in the process gas.
U. If the air demand analyzer is in service, adjust the air:acid gas ratio
as necessary with the air:acid gas manual ratio set (HIC) to bring the
air demand displayed on the air demand controller "on-scale"
(between -10.0% and +10.0%).
If the air demand is high (0.0% to +10.0%), the air:acid gas ratio is
too high (i.e., "excess air"). Reduce the setting on the air:acid gas
manual ratio set (HIC) to lower the air:acid gas ratio and reduce the
air demand.
If the air demand is low (-10.0% to 0.0%), the air:acid gas ratio is too
low (i.e., "air deficient"). Increase the setting on the air:acid gas
manual ratio set (HIC) to raise the air:acid gas ratio and increase the
air demand.
Once the air demand is "on-scale", switch the air demand controller
to "automatic" and adjust its setpoint to 0.0% air demand. the air
demand controller will now adjust the ratio setting from the air:acid
gas manual ratio set (HIC) via relays to keep a 2:1 H2S:SO2 ratio in
the tailgas leaving the SRU.
V. The sulfur plant is now on-stream, firing on amine acid gas. Before
bringing in SWS gas or directing your attention away from the SRU,
be sure that:
(3) All steam heating systems are in service and the steam traps
are functioning properly.
A. Before beginning, confirm that the following conditions are all true:
(1) SWS gas flow on/off switch in the DCS is set to "on" so that this
flow will be included in the air:acid gas ratio control system.
(2) All vent and drain valves on the SWS Gas Knock-Out Drum, its
piping, and the SWS Gas Knock-Out Drum Pump are closed
and plugged.
(3) Any blinds installed in the inlet SWS gas line have been
removed.
(4) The block valves are lined up to place a SWS Gas Knock-Out
Drum Pump in service, the H-O-A selector switch on that pump
is set to "AUTO", and the pump level control transmitter is in
service.
B. At this time, the bypass amine acid gas flow ratio controller in the
DCS is in "manual" with its output set to 0%. As a result, the bypass
acid gas control valve is closed, forcing all of the amine acid gas to
flow to the Acid Gas Burner.
D. Confirm that the setpoint of the bypass acid gas flow ratio controller
is tracking its current reading (which should be zero), then switch it to
"automatic".
E. Slowly raise the ratio setpoint on the bypass acid gas flow ratio
controller to begin opening the bypass acid gas control valve and
bypassing some of the amine acid gas to the side injection ports on
the furnace.
This should begin to raise the temperature in the front zone of the
furnace.
F. Continue to raise the ratio setpoint on the bypass acid gas flow ratio
controller until the temperature indicated on the front zone
temperature controller is approximately 1200°C.
G. It may become necessary for the bypass acid gas flow ratio controller
to "pinch" flow control valve on the amine acid gas to the acid gas
burner in order to obtain enough bypass acid gas flow through the
bypass acid gas control valve.
After the bypass acid gas flow ratio controller is controlling the
bypass acid gas flow and the furnace temperature is up to about
1200°C, the furnace is ready to accept SWS gas.
H. Slowly increase the output from the SWS gas flow control (HIC) on
the local SRU control panel to begin opening the SWS gas inlet valve
using the flow indicator on the local SRU control panel to monitor the
SWS gas flow rate.
I. As SWS gas begins flowing to the Acid Gas Burner, the air:acid gas
ratio control system will begin sending additional process air to the
burner to combust the SWS gas. Increase the SWS gas flow slowly
to allow time for the ratio control system to adjust to the increasing
SWS gas flow.
J. Continue to slowly increase the output from the SWS gas flow control
(HIC) to 100% so that the SWS gas inlet valve is fully open.
K. Monitor the bypass acid gas flow ratio controller to verify that it
maintains control of the bypass acid gas flow and that the front zone
temperature in the Reactor Furnace remains about 1200°C.
L. Observe the air demand controller and adjust the air:acid gas ratio
with the air:acid gas manual ratio set (HIC) if necessary to help keep
the air demand "on-scale".
If the air demand is high (0.0% to +10.0%), reduce the output from
the air:acid gas manual ratio set (HIC) to lower the ratio and reduce
the air demand.
If the air demand is low (-10.0% to 0.0%), increase the output from
the air:acid gas manual ratio set (HIC) to raise the ratio and increase
the air demand.
(1) Confirm that the remote ratio setpoint that the front zone
temperature controller is supplying to the bypass ratio controller
matches the current setting on the ratio controller.
(3) Switch the bypass acid gas flow ratio controller to "cascade" so
that the temperature controller can now adjust the ratio setpoint
on the ratio controller.
(5) Verify that the bypass acid gas flow ratio controller is adjusting
the bypass gas flow rate as needed to control the desired
temperature setting on the front zone temperature controller.
N. The sulfur plant is now fully on-stream, firing on both amine acid gas
and SWS gas. Before switching the SRU tailgas to the TGCU or
directing your attention away from the SRU, be sure that:
(3) All steam heating systems are in service and the steam traps
are functioning properly.
(2) The air demand indicated on the air demand controller is +2.0%
or lower.
If the air demand is higher than this, the SRU tailgas contains
excessive amounts of SO2 and could cause overheating of the
TGCU Reactor in the TGCU.
If any of these conditions are not true, do not attempt to bring SRU tailgas
into the TGCU. In particular, do not attempt switching tailgas to the TGCU
when the sulfur plant is upset. The result will be two upset units to deal
with. Instead, focus your attention on stabilizing the operation of the SRU
first (usually by correcting a problem in the upstream Amine Regeneration
Unit and/or Sour Water Stripper Unit). Then use the operating procedures
for the TGCU in Section 11 of these guidelines to switch the SRU tailgas
from flowing to the Thermal Oxidizer to flowing into the TGCU.
Once the sulfur plant tailgas is flowing to the TGCU, be sure of the
following before directing your attention away from the SRU:
(1) The Tailgas Valve to the TTO and the TGCU Warmup/Bypass
Valve are fully closed.
(5) All steam heating systems are in service and the steam traps
are functioning properly.
(6) The TGCU and the Thermal Oxidizer are functioning properly.
NOTE
(2) If any of the flanged connections in the SRU were opened for
maintenance or other purposes while the SRU was off-line, it is
good practice to leak test the SRU before returning it to service.
Refer to Section 9.7.3 of this manual for a suggested procedure
to accomplish this.
(3) Place all steam heating systems in service. Check all steam
traps for proper operation, and use the vent valves to sweep
non-condensibles out of the steam spaces.
(5) Check all devices activated by the SRU ESD system to ensure
that they operate properly.
(6) Confirm that both boilers (Waste Heat Boiler and Sulfur
Condenser) are filled with water up to their normal liquid levels.
(7) If the furnace temperature is less than 250°C, insert the startup
thermocouple assembly furnished with the optical pyrometer by
swinging the pyrometer out of the way, removing the viewport,
and attaching the thermocouple adapter to the mounting plate.
B. Confirm that the manual block valve in the SRU tailgas line is
open.
C. Confirm that the amine acid gas flow on/off switch is set to "on".
F. Place the air demand controller in "manual" and set its output to
50%.
G. Confirm that the manual signal bias control for the blower to be
used is set to 100%.
H. Select local manual control for the fuel gas flow control valve by
switching the main fuel gas hand switch (HS) in the DCS to
"local".
J. Confirm that the fuel gas flow on/off switch is set to "on".
L. Place the bypass acid gas flow controller in "manual" and set its
output to 0%.
M. Confirm that Acid Gas Firing switch on the local SRU control
panel is set to "DISABLED".
N. Confirm that Leak Test key switch on the local SRU control
panel is set to "NORMAL".
P. Set the amine acid gas flow control (HIC) and the SWS gas flow
control (HIC) on the local SRU control panel to 0% output.
Visually confirm that the amine acid gas inlet valve and the
SWS gas inlet valve are closed. If either of these valves is not
closed, H2S will be routed directly to the Thermal Oxidizer when
the Warmup Bypass Valves are opened. This could cause
overheating of the Thermal Oxidizer.
Q. Set the manual fuel gas control on the local SRU control panel
to 0% output.
Visually confirm that the main fuel gas valve and the two
shutdown valves are closed.
R. Set the air flow control (HIC) on the local SRU panel to 0%
output.
S. Verify that the acid gas control valve in the amine acid gas line
to the burner is fully open.
T. Verify that the bypass acid gas control valve in the bypass acid
gas line is fully closed.
The PLC will open the two Warmup Bypass Valves and close
the Tailgas Valve to the TTO and the Tailgas Valve to the
TGCU. Verify that the "WARMUP OPEN" light on the panel is now
illuminated and the "TTO OPEN" and "TGCU OPEN" lights on the
panel are extinguished.
B. Verify that the local start/stop controls for the Process Air
Blowers have their selector switches turned to the "STOP"
position.
(2) Start the blower using the local start/stop control station for
that blower.
E. Confirm that the air blower is running, then press the "ESD
RESET" push-button on the local SRU control panel to reset the
SRU ESD and extinguish the "RESET REQUIRED" light. This will
illuminate the "PURGE REQUIRED" light.
(1) The manual block valve(s) in the main fuel gas supply line.
(2) The manual block valve(s) in the fuel gas supply line to the
burner.
(3) The manual block valve(s) in the fuel gas supply to the
pilot.
H. Adjust the output of the air flow control (HIC) on the local SRU
panel to open the blower control valves and allow a large air
flow, 80% or more the flow indicator, to purge the furnace for 30
seconds and extinguish the "PURGE REQUIRED" light. The
"PURGE COMPLETE" light will then be illuminated.
I. Adjust the output of the air flow control (HIC) on the local SRU
panel to reduce the air flow to 10-20%, extinguishing the
"PURGE COMPLETE" light and illuminating the "PERMIT TO IGNITE"
light.
M. After the pilot is lit, use the air flow control (HIC) on the local
SRU panel to increase the air flow rate to about 50% of scale,
or as high a rate as can be maintained without blowing the pilot
out.
N. Open the vent valves on each of the two boilers to vent air from
the steam sections.
O. The heat input from the pilot will be sufficient during the early
part of the refractory warmup schedule. If the temperature is
rising too quickly, increase the air flow rate. If the temperature
is rising too slowly, decrease the air flow rate.
B. Confirm that the manual block valve(s) in the main fuel gas line
to the burner is open.
C. If the air flow rate is not at 50% of scale, use the air flow control
(HIC) on the local SRU panel to set the air flow at about 50% of
scale.
D. Press the "FUEL GAS ON" push-button on the local SRU control
panel to open the main fuel gas block valves and illuminate the
“FUEL GAS ON” light.
E. Adjust the output of the main fuel gas flow control (HIC) on the
local control panel to slowly open the control valve to
commence fuel gas flow to the warmup burner ring. Adjust the
fuel gas flow rate until a stable flame can be maintained.
F. Adjust the fuel gas flow rate with the main fuel gas flow control
(HIC) as necessary to cause the furnace temperature to follow
the refractory warmup schedule for normal warmup.
This will fully open the valves in the condensate outlet lines
from the reheat exchangers and ensure that the Reactor feeds
are as hot as possible when the switch to acid gas firing is
made.
Once the first "hold" point in the warmup schedule has been
reached, the optical pyrometer can be placed in service. After
the furnace temperature has stabilized, slide the thermocouple
out until the "keepers" stop them, close the pyrometer block
valve, then unscrew the adapter housing and store them in a
safe place.
(4) All vent and drain valves on the Acid Gas Knock-Out
Drum, its piping, and the Acid Gas Knock-Out Drum Pump
are closed and plugged.
B. Confirm that the bypass acid gas flow ratio controller in the
DCS is still in "manual" with its output set to 0%.
C. Verify that the bypass acid gas control valve is fully closed.
D. Verify that the acid gas control valve in the amine acid gas line to
the Acid Gas Burner is fully open.
E. Adjust the process air flow rate to 50% of scale on the local
indicator using the air flow control (HIC) on the local SRU panel.
Reduce the fuel gas flow rate to 50% of scale on the local
indicator using the main fuel gas flow control (HIC) on the local
panel.
WARNING
The PLC will open the Tailgas Valve to the Thermal Oxidizer
then close the Warmup Bypass Valves. The "TTO OPEN" light will
be illuminated, then the "WARMUP OPEN" light will be extinguished
as the valves move to their new positions.
G. Switch the Acid Gas Firing selector switch on the local SRU
control panel to "ENABLED".
H. Increase the output from the amine acid gas flow control (HIC)
on the local SRU control panel to begin opening the amine acid
gas inlet valve until the acid gas flow rate is approximately 10%
on the local indicator.
I. As soon as the acid gas flow rate reaches 10%, use the main
fuel gas flow control (HIC) to reduce the fuel gas flow rate from
50% to 40% on the local indicator.
L. Continue to slowly increase the output from the amine acid gas
flow control (HIC) to 100% so that the amine acid gas inlet
valve is fully open.
M. If the amine acid gas flow rate (in percent) displayed on the
local control panel is significantly different from the air flow rate
(in percent) displayed on the local control panel, use the air flow
control (HIC) on the local SRU panel to adjust the air flow until
the percentages are about the same.
(1) The two manual block valve(s) in the main fuel gas line.
(2) The manual block valve(s) in the fuel gas to the pilot.
O. Loosen the packing gland on the pilot and retract or extract the
pilot assembly:
(c) Verify that the pilot burner is still being purged with
nitrogen.
(b) Close the block valve to isolate the pilot from the
furnace.
(3) Verify that the pilot burner mounting nozzle is still being
purged with nitrogen.
(2) Confirm that the process air flow controller in the DCS is in
"cascade", its output is tracking the output of the air flow
control (HIC) on the local SRU control panel, and its
setpoint is tracking its current reading.
(4) Switch the process air hand switch (HS) from "local" to
"remote" to give the process air flow controller in the DCS
control of the Process Air Blower, so that the process air
flow rate will be ratio-controlled automatically. The output
from the air:acid gas manual ratio set (HIC) will remain fixed
at its last value.
Q. Adjust the air:acid gas ratio as necessary with the air:acid gas
manual ratio set (HIC) to bring the air demand displayed on the
air demand controller "on-scale" (between -10.0% and +10.0%).
If the air demand is high (0.0% to +10.0%), the air:acid gas ratio
is too high (i.e., "excess air"). Reduce the setting on the air:acid
gas manual ratio set (HIC) to lower the air:acid gas ratio and
reduce the air demand.
If the air demand is low (-10.0% to 0.0%), the air:acid gas ratio
is too low (i.e., "air deficient"). Increase the setting on the
air:acid gas manual ratio set (HIC) to raise the air:acid gas ratio
and increase the air demand.
(3) All steam heating systems are in service and the steam
traps are functioning properly.
A. Check that all vent and drain valves on the SWS Gas
Knock-Out Drum, its piping, and the SWS Gas Knock-Out Drum
Pump are closed and plugged.
C. Confirm that the SWS gas flow on/off switch in the DCS is set to
"on".
E. Confirm that the setpoint of the bypass acid gas flow ratio
controller is tracking the current reading (which should be zero),
then switch it to "automatic".
F. Slowly raise the ratio setpoint on the bypass acid gas flow ratio
controller to begin opening the bypass acid gas control valve
and bypassing some of the amine acid gas to the side injection
ports on the furnace.
G. Continue to raise the ratio setpoint on the bypass acid gas flow
ratio controller until the front zone temperature indicated on the
front zone temperature controller is approximately 1200°C.
After the bypass acid gas flow ratio controller is controlling the
bypass acid gas flow and the furnace temperature is up to
about 1200°C, the furnace is ready to accept SWS gas.
H. Slowly increase the output from the SWS gas flow control (HIC)
on the local SRU control panel to begin opening the SWS gas
inlet valve.
I. As SWS gas begins flowing to the Acid Gas Burner, the air:acid
gas ratio control system will begin sending additional process
air to the burner to combust the SWS gas. Increase the SWS
gas flow slowly to allow time for the ratio control system to
adjust to the increasing SWS gas flow.
J. Continue to slowly increase the output from the SWS gas flow
control (HIC) to 100% so that the SWS gas inlet valve is fully
open.
K. Monitor the bypass acid gas flow ratio controller to verify that it
maintains control of the bypass acid gas flow and that the front
zone temperature in the Reactor Furnace remains about
1200°C.
L. Observe the air demand controller and adjust the air:acid gas
ratio with the air:acid gas manual ratio set (HIC) if necessary to
help keep the air demand "on-scale".
(1) Confirm that the remote ratio setpoint that the temperature
controller is supplying to the bypass acid gas flow ratio
controller matches the current setting on the ratio
controller.
(4) Verify that the controllers are adjusting the bypass gas
flow rate as needed to control the desired temperature in
the front zone of the Reactor Furnace.
N. The sulfur plant is now fully on-stream, firing on both amine acid
gas and SWS gas. Before switching the SRU tailgas to the
TGCU or directing your attention away from the SRU, be sure
that:
(2) The air demand indicated on the air demand controller is +2.0%
or lower.
If any of these conditions are not true, do not attempt to bring SRU
tailgas into the TGCU. In particular, do not attempt switching tailgas
to the TGCU when the sulfur plant is upset. The result will be two
upset units to deal with. Instead, focus your attention on stabilizing
the operation of the SRU first (usually by correcting a problem in the
upstream Amine Regeneration Unit and/or Sour Water Stripper Unit),
and then use the operating procedures for the TGCU in the TGCU
Section of these guidelines to switch the SRU tailgas from flowing to
the Thermal Oxidizer to flowing into the TGCU.
Once the sulfur plant tailgas is flowing to the TGCU, be sure of the
following before directing your attention away from the SRU:
(1) The Tailgas Valve to the Thermal Oxidizer and the TGCU
Warmup/Bypass Valve are fully closed.
(4) All steam heating systems are in service and the steam traps
are functioning properly.
(5) The TGCU and the Thermal Oxidizer are functioning properly.
B. Confirm that the amine acid gas flow on/off switch is set to "on".
E. Place the air demand controller in "manual" and set its output to
50%.
F. Confirm that the manual signal bias control for the blower to be
used is set to 100%.
G. Select local manual control for the fuel gas flow control valve by
switching the main fuel gas hand switch (HS) in the DCS to
"local".
I. Confirm that the fuel gas flow on/off switch is set to "on".
K. Place the bypass acid gas flow controller in "manual" and set its
output to 0%.
L. Confirm that Acid Gas Firing switch on the local SRU control
panel is set to "DISABLED".
M. Confirm that Leak Test switch on the local SRU control panel is
set to "NORMAL".
O. Set the amine acid gas flow control (HIC) and the SWS gas flow
control (HIC) on the local SRU control panel to 0% output.
Visually confirm that the amine acid gas inlet valve and the
SWS gas inlet valve are closed.
P. Set the manual fuel gas control on the local SRU control panel
to 0% output.
Visually confirm that the main fuel gas valve and the two
shutdown valves are closed.
Q. Set the air flow control (HIC) on the local SRU panel to 0%
output.
R. Verify that the acid gas control valve in the amine acid gas line
to the burner is fully open.
S. Verify that the bypass acid gas control valve in the bypass acid
gas line is fully closed.
block valve in the purge nitrogen and confirm that the pilot
burner and pilot mounting nozzle are both being purged with
nitrogen.
The PLC will open the two Warmup Bypass Valves and close
the Tailgas Valve to the TTO and the Tailgas Valve to the
TGCU. Verify that the "WARMUP OPEN" light on the panel is now
illuminated and the "TTO OPEN" and "TGCU OPEN" lights on the
panel are extinguished.
B. Verify that the local start/stop controls for the Process Air
Blowers have their selector switches turned to the "STOP"
position.
(2) Start the blower using the local start/stop control station for
that blower.
E. Confirm that the air blower is running, then press the "ESD
RESET" push-button on the local SRU control panel to reset the
SRU ESD and extinguish the "RESET REQUIRED" light. This will
illuminate the "PURGE REQUIRED" light.
(1) The manual block valve(s) in the main fuel gas supply line.
(2) The manual block valve(s) in the fuel gas supply line to the
burner.
(3) The manual block valve(s) in the fuel gas supply to the
pilot.
H. Adjust the output of the air flow control (HIC) on the local SRU
panel to open the blower control valves and allow a large air
flow, 80% or more to purge the furnace for 30 seconds and
extinguish the "PURGE REQUIRED" light. The "PURGE COMPLETE"
light will then be illuminated.
I. Adjust the output of the air flow control (HIC) on the local SRU
panel to reduce the air flow to 10-20%, extinguishing the
"PURGE COMPLETE" light and illuminating the "PERMIT TO IGNITE"
light.
WARNING
The PLC will open the Tailgas Valve to the Thermal Oxidizer
then close the Warmup Bypass Valves. The "TTO OPEN" light will
be illuminated, then the "WARMUP OPEN" light will be extinguished
as the valves move to their new positions.
C. Immediately increase the output from the amine acid gas flow
control (HIC) on the local SRU control panel to begin opening
the amine acid gas inlet valve. Establish an amine acid gas
flow rate of approximately 10% and observe if ignition of the
acid gas is accomplished.
D. Increase the air flow on by 10% using the air flow control (HIC)
on the local SRU panel, then increase the amine acid gas flow
by 10%. Continue to make incremental increases in air and
amine acid gas flow, keeping about a 1:1 ratio of air to amine
acid gas (as measured by the percentages displayed on the
local indicators), until the amine acid gas inlet valve is fully
open.
(1) The two manual block valve(s) in the main fuel gas line.
(2) The manual block valve(s) in the fuel gas to the pilot.
G. Loosen the packing gland on the pilot and retract or extract the
pilot assembly:
(c) Verify that the pilot burner is still being purged with
nitrogen.
(b) Close the block valve to isolate the pilot from the
furnace.
(3) Verify that the pilot burner mounting nozzle is still being
purged with nitrogen.
(2) Confirm that the process air flow controller in the DCS is in
"cascade", its output is tracking the output of the air flow
control (HIC) on the local SRU panel and its setpoint is
tracking its current reading.
(4) Switch the process air hand switch (HS) from "local" to
"remote" to give the process air flow controller in the DCS
control of the Process Air Blower, so that the process air
flow rate will be ratio-controlled automatically. The output
from the air:acid gas manual ratio set (HIC) will remain fixed
at its last value.
I. Adjust the air:acid gas ratio as necessary with the air:acid gas
manual ratio set (HIC) to bring the air demand displayed on the
air demand controller "on-scale" (between -10.0% and +10.0%).
If the air demand is high (0.0% to +10.0%), the air:acid gas ratio
is too high (i.e., "excess air"). Reduce the setting on the air:acid
gas manual ratio set (HIC) to lower the air:acid gas ratio and
reduce the air demand.
If the air demand is low (-10.0% to 0.0%), the air:acid gas ratio
is too low (i.e., "air deficient"). Increase the setting on the
air:acid gas manual ratio set (HIC) to raise the air:acid gas ratio
and increase the air demand.
(3) All steam heating systems are in service and the steam
traps are functioning properly.
A. Confirm that the SWS gas flow on/off switch in the DCS is set to
"on".
C. Confirm that the setpoint of the bypass acid gas flow ratio
controller is tracking its current reading (which should be zero),
then switch it to "automatic".
D. Slowly raise the ratio setpoint on the bypass acid gas flow ratio
controller to begin opening the bypass acid gas control valve
and bypassing some of the amine acid gas to the side injection
ports on the furnace.
E. Continue to raise the ratio setpoint on the bypass acid gas flow
ratio controller until the front zone temperature indicated on the
front zone temperature controller is approximately 1200°C.
After the bypass acid gas flow ratio controller is controlling the
bypass acid gas flow and the furnace temperature is up to
about 1200°C, the furnace is ready to accept SWS gas.
F. Slowly increase the output from the SWS gas flow control (HIC)
on the local SRU control panel to begin opening the SWS gas
inlet valve.
G. As SWS gas begins flowing to the Acid Gas Burner, the air:acid
gas ratio control system will begin sending additional process
air to the burner to combust the SWS gas. Increase the SWS
gas flow slowly to allow time for the air flow control system to
adjust to the increasing SWS gas flow.
H. Continue to slowly increase the output from the SWS gas flow
control (HIC) to 100% so that the SWS gas inlet valve is fully
open.
I. Monitor the bypass acid gas flow ratio controller to verify that it
maintains control of the bypass acid gas flow and that the front
zone temperature in the Reactor Furnace remains about
1200°C.
J. Observe the air demand controller and adjust the air:acid gas
ratio with the air:acid gas manual ratio set (HIC) if necessary to
help keep the air demand "on-scale".
(1) Confirm that the remote ratio setpoint that the front zone
temperature controller is supplying to the bypass acid gas
flow ratio controller matches the current setting on the ratio
controller.
(4) Verify that the controllers are adjusting the bypass gas
flow rate as needed to control the desired temperature in
the front zone of the Reactor Furnace.
L. The sulfur plant is now fully on-stream, firing on both amine acid
gas and SWS gas. Before switching the SRU tailgas to the
TGCU or directing your attention away from the SRU, be sure
that:
(3) All steam heating systems are in service and the steam
traps are functioning properly.
(2) The air demand indicated on the air demand controller is +2.0%
or lower.
If any of these conditions are not true, do not attempt to bring SRU
tailgas into the TGCU. In particular, do not attempt switching tailgas
to the TGCU when the sulfur plant is upset. The result will be two
upset units to deal with. Instead, focus your attention on stabilizing
the operation of the SRU first (usually by correcting a problem in the
upstream Amine Regeneration Unit and/or Sour Water Stripper Unit),
and then use the operating procedures for the TGCU in the TGCU
section of these guidelines to switch the SRU tailgas from flowing to
the Thermal Oxidizer to flowing into the TGCU.
Once the sulfur plant tailgas is flowing to the TGCU, be sure of the
following before directing your attention away from the SRU:
(1) The Tailgas Valve to the Thermal Oxidizer and the TGCU
Warmup/Bypass Valve are fully closed.
(4) All steam heating systems are in service and the steam traps
are functioning properly.
(5) The TGCU and the Thermal Oxidizer are functioning properly.
It turns out that the process air flow rate to the SRU is actually a very good
indicator of the mass flow rate through the SRU, because the process air
flow rate is a function of the amount of combustible compounds in the
incoming feed streams. As a result, regardless of whether or not
supplemental fuel gas is being fired in the SRU, the mass flow rate
through the plant is about the same per unit of air flow. So, if action is
taken to keep the process air flow rate high, sulfur "fog" formation should
not be a problem. The action to take if the air flow drops below this point
is to begin firing supplemental fuel gas. Since burning fuel gas in the Acid
Gas Burner will require more process air to combust the fuel gas, the fuel
gas flow rate can be adjusted to maintain a minimum process air flow
(determined from experience).
The required fuel gas flow rate can be estimated from operating
experience. Once the fuel gas flow has been set using the flow control in
the DCS, observe the process air flow rate on the process air flow
controller in the DCS and adjust the fuel gas flow rate as needed to keep
the process air flow rate at the minimum flow rate. If the process air flow
is too low, raise the setpoint on the fuel gas flow controller to increase the
firing rate, which will increase the process air flow rate. If the process air
flow rate is higher than the minimum, reduce the setpoint on the fuel gas
flow controller to reduce the firing rate and reduce the process air flow.
The bypass acid gas flow ratio controller, will initially be able to maintain
the desired furnace temperature by reducing the bypass gas flow rate to
send more of the amine acid gas to the burner, which will lower the
temperature in the front zone of the Reactor Furnace. In fact, if enough
supplemental fuel gas is fired at the burner, all of the amine acid gas can
be routed to the burner due to the increase in furnace temperature caused
by the heat release from the fuel gas combustion. However, once the
bypass acid gas flow ratio controller has routed all of the amine gas to the
burner, it will no longer be able to control the front zone temperature, and
this temperature may begin to rise. If so, reduce the supplemental fuel
gas flow rate as needed to keep the furnace temperature below 1,500°C
(preferably, below 1370°C).
A. Select local manual control for the fuel gas flow control valve by
switching the main fuel gas hand switch (HS) in the DCS to
"local".
C. If necessary, "toggle" the fuel gas flow on/off switch in the DCS
to "ON" so that the fuel gas flow will be included in the
air:acid gas ratio control system.
D. Set the manual fuel gas control on the local SRU control panel
to 0% output and visually confirm that the main fuel gas valve
and the two shutdown valves are closed.
(1) The upstream manual block valve(s) in the main fuel gas
supply line.
F. Press the "FUEL GAS ON" push-button on the local SRU control
panel to open the main fuel gas block valves and illuminate the
“FUEL GAS ON” light.
G. Adjust the output of the main fuel gas flow control (HIC) on the
local SRU control panel to slowly open the control valve and
commence fuel gas flow to the warmup burner ring. Look
through the viewports on the Acid Gas Burner and adjust the
fuel gas flow rate until a stable flame can be maintained on the
burner tips.
H. Observe the air flow on the process air flow controller and
confirm that the air:acid gas ratio control system has added the
air needed to combust the fuel gas.
(1) Confirm that the fuel gas flow controller in the DCS is in
"automatic", its output is tracking the output of the main
fuel gas flow control (HIC) on the local SRU control as
indicated in the DCS, and its setpoint is tracking its current
reading.
(2) Switch the main fuel gas hand switch (HS) from "local" to
"remote". The DCS controller now has control of the fuel
gas control valve and will be controlling a fixed fuel gas
flow rate, with its setpoint equal to the last reading
If necessary, lower the fuel gas flow rate to keep the furnace
temperature at 1,500°C or below. Once the output from the
bypass acid gas flow ratio controller reaches 0% and the
bypass acid gas control valve is fully closed, the bypass gas
ratio controller will no longer be able to control the furnace
temperature.
M. Monitor the air demand on the air demand controller closely and
be prepared to adjust the air:acid gas ratio as necessary with
the air:acid gas manual ratio set (HIC) to help the air demand
controller keep the plant "on-ratio".
N. If the warmup burner does not light or will not maintain a stable
flame:
(1) Press the “FUEL GAS OFF” push button to block-in the main
fuel gas.
(2) Verify that the main fuel gas automated block valves have
closed, the main fuel gas automated vent valve has
opened, and the “FUEL GAS ON” light has been
extinguished.
(3) Close the manual block valve(s) in the main fuel gas
supply line.
B. Slowly reduce the output from the fuel gas flow controller to 0%
to close the control valve in the main fuel gas line and reduce
the fuel gas flow to zero. Lower the fuel gas flow rate slowly to
allow the air:acid gas ratio control system to adjust the air flow
properly.
C. Press the “FUEL GAS OFF” push-button on the local SRU control
panel to "double block and bleed" the main fuel gas.
D. Verify that the main fuel gas block valves have closed, the
“FUEL GAS ON” light has been extinguished, and the warmup
burner is being purged with nitrogen.
E. Close the two manual block valve(s) in the main fuel gas line.
F. "Toggle" the fuel gas flow on/off switch in the DCS to "OFF" so
that the fuel gas flow rate will no longer be included in the
air:acid gas ratio control system (in case the meter does not
read exactly zero when there is no flow).
Also, Section 9.9.1.K (1) briefly addresses keeping a sulfur plant on hot
stand-by to minimize corrosion due to water condensation in the boiler and
exchanger tubes. Since each SRU has a warmup bypass line to the Thermal
Oxidizer, they can be kept on hot stand-by indefinitely by firing on fuel gas and
venting the combustion products to the Thermal Oxidizer. This allows
maintaining the furnace refractory and heat exchanger surfaces at their normal
operating temperatures, ready to accept acid gas, without exposing the catalyst
beds to overheating, carbon deposition, or sulfation damage. (Refer to the
description of cold catalyst bed startup in these guidelines.)
One special circumstance that may exist during a shutdown is to have tube
leaks in either the Waste Heat Boiler or the Sulfur Condenser. This special
case is discussed in Section 9.9.3.
Each SRU is affected directly and indirectly by shutdowns and outages that
occur in other systems. The more important aspects of the effects these other
systems can have on the SRUs are discussed in Section 9.9.5.
Typical shutdown procedures are outlined and discussed in the sections that
follow for the more common cases. Your existing company procedures and
common sense operational judgment should be used to modify these
procedures as needed to serve the purpose of any given planned shutdown
situation.
To shut the SRU down in a controlled fashion, follow the procedure below.
However if one SRU remains on-line, the TGCU can remain online
as well.
B. Discontinue SWS gas flow to the SRU by slowly reducing the output
from the manual control hand controller on the local SRU control
panel to begin closing the SWS gas shutdown valve. Allow time for
the air flow controller to reduce the air flow to the SRU accordingly.
D. Begin to "back out" the amine acid gas flow to the SRU by slowly
reducing the output from the manual control hand controller on the
local SRU control panel to begin closing the amine acid gas
shutdown valve. Allow time for the air flow controller to reduce the
air flow to the SRU accordingly.
E. Observe the amine acid gas flow rate the flow indicator on the local
SRU control panel and continue reducing the output on the manual
controller until the flow rate drops to 20-30%.
The pressure control system on the stripper in the ARU should begin
to divert the amine acid gas flow to the flare as the feed rate to the
SRU is reduced.
F. Once the amine acid gas flow rate is down to 20-30%, the SRU can
be shut down with minimal impact on the other process units. The
simplest way to do so is to activate the SRU ESD system, using
either the push-button in the DCS or the push-button on the local
SRU control panel.
(3) The fuel gas to the Acid Gas Burner is blocked-in and bled.
(4) The Process air Blower is shut down and the suction, blow-off,
and discharge valves are closed.
(5) All steam heating services are still functioning and the steam
traps are operating properly.
H. If the TGCU was shut down in Step A, the Tailgas Valve to the TTO
should have been opened and the Tailgas Valve to the TGCU should
have been closed automatically. Visually confirm the positions of
these valves.
(1) Switch the Startup/Run selector switch on the local SRU control
panel to "STARTUP".
The PLC will open the two Warmup Bypass Valves and close
the Tailgas Valve to the TGCU. Verify that the "WARMUP OPEN"
light on the panel is now illuminated and the "TGCU OPEN" light
is extinguished.
The PLC will open the Tailgas Valve to the TTO, then close the
Warmup Bypass Valves. Verify that the "TTO OPEN" light on the
panel is illuminated, and that the "WARMUP OPEN" and "TGCU
OPEN" lights are extinguished.
I. If the other SRU and the TGCU are to remain online, isolate the
off-line SRU from the TGCU and the Thermal Oxidizer:
(6) Switch the Startup/Run selector switch on the local SRU control
panel to "STARTUP".
(7) The PLC will open the two Warmup Bypass Valves and close
the Tailgas Valve to the TGCU or the Tailgas Valve to the TTO.
Verify that the "WARMUP OPEN" light on the panel is now
illuminated and the "TTO OPEN" and "TGCU OPEN" lights on the
panel are extinguished.
(8) Turn the Leak Test key switch on the local SRU control panel to
"TEST".
(9) The PLC will close the two Warmup Bypass Valves and start the
nitrogen purge between the valves. Verify that the "WARMUP
OPEN" light on the panel is now extinguished, and that nitrogen is
flowing into the piping by observing the FI.
(10) If desired, close the manual block valve in the SRU tailgas line.
WARNING
(1) The Waste Heat Boiler, the reheat exchangers and the Sulfur
Condenser can be kept hot by firing the warmup burner in the
Acid Gas Burner with fuel gas, using the Warmup Bypass
Valves to divert the combustion gases to the Thermal Oxidizer.
Use the procedures in these guidelines to fire the SRU in hot
standby mode on fuel gas.
(2) If this is not possible, allow the two boilers to cool enough to
reduce the steam pressure to about 1 kg/cm2(g). Then
de-pressure the boilers and drain the water from them. Use a
temporary "jumper" to supply LP steam to the Waste Heat
In this procedure, where complete cooling of the plant and air purging are
required, the time-controlling step will be the period of time required to
cool the catalyst beds below 150°C. Also, attention should be given to the
cooling of the Reactor Furnace refractory; it should be limited to
100-150°C per hour. The catalyst beds must be cooled to 150°C or below
before air flow can be established to purge the plant and cool it rapidly
from that temperature. If the catalyst beds are not cooled to this level
before beginning the air purge, sulfur fires can occur in the beds, the
sulfur separators and mist eliminators, and the other parts of the plant
where elemental sulfur is present.
heaters.) This will keep the tubes in the boilers and reheat
exchangers safely above the water condensation temperature
(100-110°C).
The preferred source of inert gas is nitrogen from the plant header. If
nitrogen (or some other type of inert gas from an external source) is
available in sufficient quantity, follow the procedure given in this
section to use nitrogen or inert gas as the stripping media.
(3) The fuel gas to the Acid Gas Burner is blocked-in and
bled.
(4) The Process air Blower is shut down and the suction,
blow-off, and discharge valves are closed.
(7) The manual block valve in the SRU tailgas line is open.
(8) All steam heating services are still functioning and the
steam traps are operating properly.
(1) If using nitrogen from the plant header, the nitrogen can be
introduced through the hard-piped connection on the
process air line near the Acid Gas Burner.
The hot inert gas flowing through the Reactor should vaporize
most of the residual sulfur contained in the catalyst beds so that
it can be condensed and removed in the downstream
condensing passes of the Sulfur Condenser.
E. Continue to purge the sulfur plant with this inert gas stream until
sulfur is no longer running from any of the Sulfur Drain Seal
Assemblies.
Once sulfur stops running from all of the Sulfur Drain Seal
Assemblies, cool-down of the catalyst beds can commence
using the procedure given in Section 9.9.2.3 that follows.
(1) If dry inert gas (nitrogen) is being used for the cooling gas,
the steam pressures in both boilers can be allowed to fall
to 0 kg/cm2(g), since there is no risk of water condensation
in the tubes.
(2) If the warmup burner in the Acid Gas Burner is being used
to generate the inert gas, it may not be possible to reduce
the Waste Heat Boiler steam pressure to
C. Monitor the water levels in the Waste Heat Boiler and the Sulfur
Condenser and confirm that the level controls continue to
function properly to maintain normal levels in the boilers
throughout the cool-down procedure.
(1) Route nitrogen, steam, or some other inert gas through the
reactor.
E. When all catalyst beds are below 150°C, stop the flow of
cooling gas. Switch the Startup/Run selector switch on the
local SRU control panel to "STARTUP".
The PLC will open the two Warmup Bypass Valves and close
the Tailgas Valve to the TTO Unit. Verify that the "WARMUP
OPEN" light on the panel is now illuminated and the "TTO OPEN"
light is extinguished.
(2) Set air blower flow controller (HIC) on the local SRU
control panel to 0% output.
(4) Start the blower using the local start/stop control station for
that blower.
The PLC will open the Tailgas Valve to the TTO, then close the
Warmup Bypass Valves. Verify that the "TTO OPEN" light on the
panel is illuminated, and that the "WARMUP OPEN" and "TGCU
OPEN" lights are extinguished.
I. Increase the output from the local air flow controller (HIC) to
begin a rapid air purge of the entire sulfur plant.
CAUTION
J. Continue the rapid air purge of the entire sulfur plant until all
temperatures are approximately equal to the discharge air
temperature from the blower.
L. Once the plant is isolated from the feed gases, discontinue the
air purge by shutting down the Process Air Blower.
N. Isolate the SRU from the TGCU and the Thermal Oxidizer:
The PLC will open the two Warmup Bypass Valves and
close the Tailgas Valve to the TTO. Verify that the
(2) Turn the Leak Test key switch on the local SRU control
panel to "TEST".
The PLC will close the two Warmup Bypass Valves and
start the nitrogen purge between the valves. Verify that the
"WARMUP OPEN" light on the panel is now extinguished, and
that nitrogen is flowing into the piping by observing the FI.
(3) If desired, close the manual block valve in the SRU tailgas
line.
(1) The SRU is isolated from the amine acid gas source, the
SWS gas source, the fuel gas header, the instrument air
header, the nitrogen header, the TGCU, and the Thermal
Oxidizer.
(2) The Process Air Blowers are shut down and their suction,
blow-off, and discharge valves are closed.
(3) All steam heating services are still functioning and the
steam traps are operating properly. If possible, the
LP steam and condensate system should remain in
service, with selected branches taken out of service as
required for maintenance.
P. The plant can now be opened for entry. Refer to the "General
Safety" section of these procedures for important
considerations when performing maintenance work on this
plant.
WARNING
2. Liquid water may reach the refractory linings in the equipment and
damage the linings.
3. Water and/or steam may reach the catalyst in the Reactor and
weaken or damage it.
4. If there is a large tube leak in the Waste Heat Boiler, water may
back-flow into the hot Reactor Furnace and rapidly vaporize, possibly
violently enough to damage its refractory lining or create high
pressure in the SRU.
A. Shut down the SRU using the procedures given in Section 9.9.1.
C. De-pressure the boiler having the suspected tube leak, taking care to
reduce the pressure slowly enough to avoid over-stressing the boiler.
D. Maintain a visible water level in the boiler. Water must remain in the
boiler until it is de-pressured to prevent overheating damage to the
tubes.
E. Once the boiler is fully de-pressured, drain the water from the boiler
to prevent any further leakage into the process side of the
equipment.
F. The SRU is now ready to be isolated and made safe for entry.
Reactor 1st Bed Outlet 1. Malfunction of the air:acid gas ratio control
High-High Temperature system, allowing excess air to enter the
system.
2. Malfunction of the control system has
caused less than 1/3 of the acid gas to be
routed to the burner, allowing free oxygen
to reach the catalyst bed.
3. Low H2S concentration in the inlet acid gas
is causing incomplete combustion in the
Reactor Furnace, allowing free oxygen to
reach the catalyst bed.
4. Damaged acid gas burner tip causing
incomplete mixing and combustion of air
and acid gas, allowing free oxygen to reach
the catalyst bed.
5. Malfunction of the control system has
caused a high reactor inlet temperature.
If the interruption in the ARU is long enough, though, the amine acid
gas flow can fall far enough to cause the acid gas flame in the SRU
to become unstable, at which point the SRU ESD system will be
activated by "flame failure". If this happens, the SRU can be
restarted on fuel gas and run in hot stand-by using the Warmup
Bypass Valves, then brought back on-line once amine acid gas flow
resumes. If the SRU is currently processing SWS gas, it is possible
that the acid gas flame may remain stable enough for continued
operation on just SWS gas. If the SRU is processing only SWS gas,
note the cautions in these guidelines regarding this mode of
operation.
When the TGCU warmup/bypass valve first opens, the pressure drop
through the TGCU will no longer be imposing back-pressure on the
SRUs. Depending on the magnitude of this change in back-pressure
(which is mainly determined by the unit throughput), there may be a
temporary "bobble" in the feed and air flow rates to the SRUs.
Although this will probably cause brief deviations from the proper
air:acid gas ratio in the SRUs, the "bobble" should not be large
enough to cause a "flame failure" shutdown in the SRU. If so, the
SRU will remain on-line with its tailgas flowing to its Thermal
Oxidizer, so that there is no need to restart the SRUs. Once the
TGCU has been restarted, the SRU tailgas streams can be
reintroduced into the TGCU to resume processing with as little
interruption as possible.
TGCU effluent is low and the stack is tall, dangerous ground level
concentrations of H2S should not develop.
If the H2S concentration in the TTO feed gas is high (above 3.0%),
do not attempt to restart the Thermal Oxidizer. Instead, direct your
attention to the amine or SWS unit(s) upstream of the SRUs that are
probably causing the problem and bring the SRUs back on-ratio, so
that the H2S concentration in the Thermal Oxidizer feed gas is
reduced to an acceptable level and restart of the Thermal Oxidizer
can proceed smoothly.
The more immediate impact on the SRU will be the loss of LP steam
to the stripper reboiler in the upstream Amine Regeneration Unit if
the steam outage lasts long enough. As the heat input to the reboiler
declines, stripping of the acid gas from the solvent will decline and
the amine acid gas flow rate to the SRU will gradually diminish. If the
amine acid gas flow falls far enough to cause the acid gas flame to
become unstable, the SRU ESD system will be activated by "flame
failure" as described previously in the discussion about Amine
Regeneration Unit outages.
1. The H2S concentration in the inlet amine acid gas using Tutweiler analysis
(Sections 9.10.1, 9.10.2, 9.10.6, and 9.10.7).
2. The H2S and SO2 concentrations in the SRU tailgas using Tutweiler
analysis (Sections 9.10.1 and 9.10.3 through 9.10.7).
3. The H2S and SO2 concentrations in the SRU tailgas using gas detector
tubes (Section 9.10.8).
4. Attach the leveling bottle filled with starch solution to the lower
stopcock of the Tutweiler burette.
Raise the leveling bottle, open the lower stopcock, open the upper
stopcock to the inlet tube connection and completely fill the burette.
Close the upper stopcock when a few drops of the starch solution
flow out of the inlet tube connection. Close the lower stopcock.
7. Crack the gas sample valve open and draw gas into the burette by
lowering the leveling bottle and opening the stopcocks. When the
liquid level is several milliliters below the 100-ml mark (500-ml mark),
close the lower stopcock, upper stopcock, and gas sample valve.
8. Remove the sample gas rubber tubing from the Tutweiler burette.
9. Open the lower stopcock and bring the starch solution to the
100-ml mark (500-ml mark) by raising the leveling bottle; then close
the lower stopcock. Open the upper stopcock long enough to
equalize the pressure inside the burette with the atmosphere, then
close the top stopcock. There is now exactly 100 ml (500 ml) of gas
at atmospheric pressure and ambient temperature in the Tutweiler
burette.
10. Open the lower stopcock and lower the leveling bottle. Lower the
level of the starch solution in the burette to the 110-ml mark
(550-ml mark) to pull a partial vacuum. Close the lower stopcock.
11. Place a tubing clamp on the rubber hose to the leveling bottle and
remove the hose from the Tutweiler burette lower stopcock.
12. Carefully crack the stopcock on the iodine burette and allow a small
amount of iodine solution to be sucked into the large burette. Close
the stopcock.
13. Shake the burette vigorously, carefully holding the glass cap in place
on top of the iodine burette with one finger. As soon as all traces of
blue are gone, repeat the addition of iodine solution, adding smaller
and smaller amounts as the "anticipated" volume is approached.
14. Continue the titration until the starch solution turns a definite blue
color and holds the color without fading during shaking for
approximately one minute. Carefully read the final iodine burette
level.
15. Record the temperature of the air around the sampling point.
1. Using a 100 ml Tutweiler apparatus, sample and titrate the acid gas
feed to the SRU as outlined in Section 9.10.1.
H2S + I2 2 HI + S
The Normality of the standard iodine solution will be 0.1 N. The last
three factors (which correct the actual acid gas content to
compensate for expansion due to temperature, pressure, and water
content) can be combined and calculated as a function of
temperature only. This has been done for the 100-ml gas sample
16.0
Chart 1
15.5
Tutweiler Factor
vs.
Air Temperature
15.0
Sample Volume: 100 ml
Baro. Pressure: 1.033 kg/cm2(a)
14.5
14.0
13.5
13.0
Tutweiler Factor
12.5
12.0
11.5
11.0
10.5
10.0
9.5
9.0
H2S + I2 S + 2 HI
The hydrogen sulfide (H2S) and sulfur dioxide (SO2) are converted by
the iodine during the shaking. When both gases are completely
converted, the slightest excess of free iodine causes the
characteristic blue color with the starch solution. Although the
relative amount of each gas cannot be determined from the Tutweiler
titration alone, only sulfur dioxide is converted to sulfuric acid
(H2SO4). Therefore, a further step can be used to determine the
amount of sulfuric acid formed in order to calculate the amount of
sulfur dioxide originally present in the gas sample.
5. Add five drops of methyl purple indicator to the flask and swirl gently.
8. Calculations:
a. For a 500-ml gas sample, Mole (or Vol) percent H2S + SO2 (dry
basis):
Mole % H2S
H2S : SO2 Ratio
Mole % SO2
3.2
Chart 2
3.1
Tutweiler Factor
vs.
Air Temperature
3.0
Sample Volume: 500 ml
Baro. Pressure: 1.033 kg/cm2(a)
2.9
2.8
2.7
2.6
Tutweiler Factor
2.5
2.4
2.3
2.2
2.1
2.0
1.9
1.8
Examples:
If 3.0 ml I2 and 4.6 ml NaOH are used (these are off the table), divide
by 2 to get 1.5 ml I2 and 2.3 ml NaOH, for a molar ratio of
H2S:SO2 = 0.88.
The values in the table below are the ratio of H2S:SO2 for the quantities of
iodine and sodium hydroxide used in the titrations.
NOTE: This table is valid only when the Normalities of the iodine and
sodium hydroxide solutions are the same.
ml
I2 ml of NaOH
1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 2.0
0.9 8.00 3.50 2.00 1.25 0.80 0.50 0.28 0.12 0.00 * *
1.0 * 9.00 4.00 2.33 1.50 1.00 0.67 0.43 0.25 0.11 0.00
1.1 * * 10.00 4.50 2.67 1.75 1.20 0.84 0.58 0.38
1.2 * * * 11.00 5.00 3.00 2.00 1.40 1.01 0.73 0.51
1.3 * * * * 12.00 5.50 3.33 2.25 1.60 1.18 0.88
1.4 * * * * * 13.00 6.00 3.67 2.50 1.80 1.35
1.5 * * * * * * 14.00 6.50 4.00 2.75 2.00
1.6 * * * * * * * 15.00 7.00 4.33 3.00
1.7 * * * * * * * * 16.00 7.50 4.67
1.8 * * * * * * * * * 17.00 8.00
1.9 * * * * * * * * * * 18.00
2.0 * * * * * * * * * * *
* Erroneous Test
ml
I2 ml of NaOH
2.0 2.1 2.2 2.3 2.4 2.5 2.6 2.7 2.8 2.9 3.0 3.1
* Erroneous Test
6.0
Chart 3
5.5
Tailgas Analysis
Operating Chart
H2S:SO2 = 2.3
5.0 (Both solutions must be
the same normality)
H2S:SO2 = 1.7
4.5
4.0
DEFICIENT AIR
ml of Iodine Solution
3.0
2.5
2.0
1.5
1.0
0.5
0.0
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5
ml of Sodium Hydroxide Solution
Issued 30 August 2011 Sulfur Recovery Page 9-198
Operating Guidelines Samsung Total Petrochemicals Co., Ltd.
Fall 2011 Daesan, Korea
SULFUR BLOCK
16. Reagent bottles, plain narrow mouth, with flat head stopper, Pyrex,
1 liter capacity, three.
17. Amber bottles with Bakline screw caps, 5 pint capacity (approx.
2.5 liters), two.
9.10.8 H2S and SO2 Conc. in Tailgas Using Gas Detector Tubes
As an alternative to the traditional wet-chemistry methods described in the
preceding Section 1 for determining the concentrations of H2S and SO2 in
the sulfur plant tailgas, gas detector tubes can be used to quickly and
easily make this determination. Although the discussion that follows
specifically addresses using gas detector tubes manufactured by
Drägerwerk AG of West Germany, there may be suitable detector tubes
available from other manufacturers. Dräger tubes can be purchased from
most safety equipment supply companies.
c. Break off the tips at each end of an H2S Dräger tube and insert
it into the sample pump (with the arrow on the side of the tube
pointing toward the pump).
e. Stroke the sample pump one time (be sure to compress the
bellows until reaching the stops) and allow the pump to draw
the gas sample into the detector tube. The sample stroke is
complete when the metal chain on the bellows is taut.
f. Close the sample valve, remove the rubber tubing from the end
of the Dräger tube, and use the pump to draw two strokes of
fresh air through the detector tube to complete the reactions.
g. Read the length of the black stain using the cm marks on the
tube and record the reading.
h. Break off the tips at each end of an H2S+SO2 Dräger tube and
insert it into the sample pump (with the arrow on the side of the
tube pointing toward the pump).
j. Read the length of the yellow stain using the cm marks on the
tube and record the reading.
k. Check that the sample valve is closed, then remove the rubber
tubing.
9.10.8.3 Calculations
a. Mole (or Volume) percent H2S (wet basis):
Mole % H2S
H2S : SO2 Ratio
Mole % SO2
9.10.8.4 Example
Suppose, for example, that the following measurements are taken:
0.66%
d. H2S : SO2 Ratio = = 1.61
0.41%
This indicates that the H2S:SO2 ratio is a little low (less than 2.0), so
the air:acid gas ratio is on the high side. The output from the air
demand hand control should be lowered slightly, and the
measurements repeated after the SRU reaches a steady state again.
If the H2S:SO2 ratio had been high (greater than 2.0), that would
have meant that the air:acid gas ratio was on the low side. In that
case, the output from thr air demand hand control would need to be
raised slightly to increase the air flow and bring the H2S:SO2 ratio
down.
In order for a flame front generator to work properly, two conditions must be
satisfied. First, the air:gas mixture must be within the flammability limits (neither
too lean nor too rich). Second, the flowing velocity of the mixture must be higher
than the flame speed so that the "fireball" will travel to the pilot. The ignitor has
orifices to regulate the air and fuel gas, sized by the manufacturer to provide the
proper quantities of air and fuel gas when both streams are at the manufacturer’s
specified pressure as indicated on the pressure gauges for both air and fuel gas
supplied on the pilot assembly.
In theory, adjusting the pilot air and fuel gas regulators to the manufacturer’s
specified pressure should be all that is needed to make the ignitor work. In
practice, a certain amount of adjustment of the pressures is sometimes required
before the ignitor works reliably, especially if the fuel gas composition is variable.
However, once the proper pressures are determined, the ignitor can usually be
made to work easily by making sure that the regulators are set to these pressures
before attempting to ignite the pilot.
If the pilot does not light with the regulators set at the design pressures,
trial-and-error can be used to determine the proper regulator pressures. One
technique that has worked well is described below. It requires two operators:
one to adjust the regulators, one to control the ignition cycle and observe the pilot.
2. Unscrew the adjustment screw on the pilot fuel gas regulator so that the
pilot fuel gas is at minimum pressure.
3. Follow the procedures given in these guidelines to start the air blower and
reset the shutdown system.
4. The first operator raises the air flow (using the hand indicator controller) to
satisfy the "PURGE REQUIRED" light, lowers the air flow to get the "PERMIT
TO IGNITE", then pushes the "IGNITION" push-button to begin an ignition
attempt.
5. Once the ignition cycle starts, the second operator begins gradually
increasing the pilot fuel gas pressure from the pressure control valve
(observing the pressure on the local pressure gauge) while the first
operator observes the operation of the pilot through one of the viewports
on the burner.
6. As the pilot fuel gas pressure increases, a flame will be observed on the
pilot. When the flame is observed, the second operator should stop
increasing the pilot fuel gas pressure.
7. If the pilot does not ignite, repeat the sequence beginning at Step 4,
starting with the pilot fuel gas regulator set where it was at the end of the
previous ignition attempt, or a little lower.
9. Once a flame is observed on the pilot, the pilot fuel gas pressure can then
be adjusted to produce a good stoichiometric pilot flame. While the first
operator continues to observe the pilot flame through the burner viewport,
the second operator can raise or lower the pilot fuel gas pressure slightly
until the pilot flame is dark blue:
a. If the flame is yellow, the air:natural mixture is too "rich". Lower the
fuel gas pressure with the pressure control valve to reduce the
amount of fuel gas flowing to the pilot.
b. If the flame is light blue, the air:natural mixture is too "lean". Raise
the fuel gas pressure with the pressure control valve to increase the
amount of fuel gas flowing to the pilot.
10. Once the pilot has ignited, make note of the pilot air and fuel gas
pressures for future reference. The pilot regulators should be adjusted to
these settings prior to subsequent startups.
Table of Contents
10. SULFUR DEGASSING, STORAGE & LOADING .................................................. 10-3
10.1 PURPOSE OF SYSTEM ..................................................................................... 10-3
10.2 SAFETY ............................................................................................................... 10-4
10.3 PROCESS DESCRIPTION.................................................................................. 10-5
10.4 EQUIPMENT DESCRIPTION .............................................................................. 10-7
10.4.1 Sulfur Degassing Reactor, A2-DC1550 ........................................................ 10-7
10.4.2 Sulfur Storage Tank, A2-FB1550 ................................................................. 10-7
10.4.3 Sulfur Feed Pump, A2-GA1532A/B (A2-GA1542A/B) .................................. 10-8
10.4.4 Sulfur Loading Pump, A2-GA1550A/B ......................................................... 10-8
10.4.5 Degassing Air Blower, A2-GB1550A/B ......................................................... 10-9
10.4.6 Bed Support and Limiter for Sulfur Degassing Reactor, A2-DC1551 ........... 10-9
10.4.7 Degassed Sulfur Drain Seal Assembly, A2-ME1550.................................... 10-9
10.5 INSTRUMENTATION AND CONTROL SYSTEMS ........................................... 10-11
10.5.1 Sulfur Feed Rate Control ............................................................................ 10-11
10.5.2 Degassing Air Flow..................................................................................... 10-12
10.5.3 Sulfur Degassing Unit Startup Interlock ...................................................... 10-13
10.5.4 Snuffing Steam ........................................................................................... 10-13
10.5.5 Sulfur Loading ............................................................................................ 10-14
10.5.6 Sulfur Loading Pump Local Stop Switches................................................. 10-17
10.5.7 Sulfur Degassing Shutdown System .......................................................... 10-18
10.5.8 Sulfur Loading ESD System ....................................................................... 10-21
10.6 PROCESS PRINCIPLES AND OPERATING TECHNIQUES ........................... 10-23
10.6.1 Equipment Damage .................................................................................... 10-23
10.6.2 Degassing Air Blower Operation ................................................................ 10-26
10.6.3 Sulfur Solidification ..................................................................................... 10-29
10.6.4 Sulfur Pumping ........................................................................................... 10-29
10.7 PRECOMMISSIONING PROCEDURES ........................................................... 10-31
10.7.1 Preliminary Check-out ................................................................................ 10-31
10.7.2 Commissioning the Heating and Ventilation Systems ................................ 10-32
10.7.3 Purging the Sulfur Degassing Reactor ....................................................... 10-37
10.8 STARTUP PROCEDURES................................................................................ 10-40
10.8.1 Initial Startup of the Sulfur Degassing Unit ................................................. 10-40
10.8.2 Normal Startup of the Sulfur Degassing System ........................................ 10-46
10.8.3 Initial Sulfur Loading Operation .................................................................. 10-51
10.8.4 Normal Sulfur Loading Operation ............................................................... 10-53
10.9 SHUTDOWN PROCEDURES ........................................................................... 10-54
10.9.1 Planned Shutdown - No Reactor Entry....................................................... 10-54
The purpose of the Sulfur Storage & Loading system is to collect the degassed
sulfur, hold it in a molten state, and then load it into trucks as a product for sale.
10.2 Safety
WARNING
The liquid sulfur produced in the condensers of a Claus sulfur plant is in contact
with process gas containing hydrogen sulfide at elevated temperature and
pressure. As a result, the fresh sulfur product from Claus plants contains a
significant amount of hydrogen sulfide. Some of the hydrogen sulfide in the
sulfur is dissolved H2S gas, but the majority of it is hydrogen polysulfide (H2SX)
formed in the condensers by the following reaction:
While the liquid sulfur is stored in the Sulfur Surge Tank, a considerable portion
of the polysulfide will break down into H2S and be released into the ventilation
air circulated through the vapor space of the tank. This natural "weathering"
process typically reduces the H2S content of the molten sulfur to 50-100 PPMW
after one or more days of storage. However, since the natural decomposition of
H2SX in the liquid sulfur is a slow and generally incomplete process, additional
means of degassing the sulfur must be employed to ensure that the H2S content
of the sulfur product does not exceed 10 PPMW.
the polysulfide.
The spent degassing air (containing H2S and traces of elemental sulfur vapor)
leaves the top of the Sulfur Degassing Reactor and is routed to the TTO for
incineration.
The Sulfur Storage Tank is sized to hold about two week of production from the
two SRUs, or about 500 MT when completely full. The tank is constructed of
carbon steel and is equipped with internal steam coils and a ventilation system.
Since the normal liquid level for molten sulfur in this reactor is at the top of
the weir on the draw pan above the catalyst bed, the bottom head and
shell of the vessel are steam-jacketed. The inlet and outlet sulfur, inlet air,
outlet gas, and clean-out nozzles are also steam-jacketed.
through a 3 m tall heated vent stack, mounted on top of the tank. The
steam-jacketing on the vent stack heats the air in the stack, providing the
natural-draft driving force that draws ambient air into the tank to sweep the
vapor space.
WARNING
Both the bed support and the bed limiter are designed to have about a
12 mm gap next to the vessel shell to allow for differential thermal
expansion between the bed support and the vessel. Ceramic rope
packing is used to fill this gap so that catalyst cannot leak between the
bed support and the vessel shell.
Sulfur Tank through a drain pipe to prevent free-fall of the liquid sulfur,
which could cause static electricity to build up. The drain seal is mostly
carbon steel, except for the inspection hatch which is aluminum.
The drain seal has a removable blind flange to allow "rodding" its rundown
line, and a removable blind flange to allow "rodding" its dip leg. Before
removing either flange, close the plug valve in the rundown line to prevent
the escape of process gas to the surroundings when the plug is cleared.
When the rodding operation is complete and the flange(s) are back in
place, remember to reopen the plug valve.
at the desired value while avoiding sudden changes in the feed rate to the
Sulfur Degassing Reactor.
There are two reasons for using a fixed degassing air flow rate rather than
controlling the air:sulfur flow ratio. The first reason is that the spent
degassing air from the Sulfur Degassing Reactor is routed to the Thermal
Oxidizer as a part of its feed. Keeping the degassing air flow rate at a
constant value makes it easier to maintain good temperature control in the
TTO.
The second reason is that variations in the air flow rate can cause
fluctuations in the sulfur feed rate to the Sulfur Degassing Reactor. The
pumping rate of the Sulfur Feed Pumps depends on the discharge
pressure from the pumps, which is in turn a function of the static head
imposed on the pump discharge. This static head has two components:
the static head of the liquid sulfur in the discharge piping going to the
Sulfur Degassing Reactor, and the static head of the sulfur/air mixture in
the Sulfur Degassing Reactor. While the first static head is essentially
constant because the density of liquid sulfur is relatively constant, the
second static head depends on the density of the sulfur/air mixture in the
reactor. Small changes in the degassing air flow rate cause very large
changes in the density of the sulfur/air mixture, which then cause very
large changes in the pump discharge pressure. Field experience has
shown that the sulfur flow rate remains much steadier when the degassing
air flow rate is held at a fixed value.
If the degassing air flow rate ever drops too low (as signaled by the low
flow alarm on A2-FI15702) and the low flow condition cannot be corrected
in a reasonable length of time, the SDU should be shut down until the air
flow problem has been corrected.
The logic flowchart for the SDU "start" permissives is contained in the
Instrumentation and Controls Diagrams section of the Basic Engineering
Package. These permissives are (in order):
(1) Start a Sulfur Feed Pump.
(1) Allow the pump to fill the Sulfur Degassing Reactor to satisfy its
low-low level shutdown.
(2) Start a Degassing Air Blower and press its "reset" push-button to
open its discharge valve.
There is a snuffing steam line entering the top of the Sulfur Storage Tank
to flood the tank vapor space with LP steam in case a fire develops inside
the tank. The snuffing steam supply valve is operated by either a remote
switch in the DCS or a local switch that is located at least 50 feet from the
tank. Opening this valve for a few minutes will fill the vapor space of the
tank with steam and displace all of the air, quickly extinguishing the fire.
The logic for the snuffing steam valves is contained in the Instrumentation
and Controls Diagrams section of the Basic Engineering Package. They
can be opened by "toggling" the switch in the DCS to "on" or by pressing
the local push-button. The valve can be closed later by "toggling" the
switch in the DCS to "off" or by pressing the local push-button again.
The logic for sulfur loading operations is shown on the Logic Flow
Diagrams contained in the Instrumentation and Controls Diagrams section
of the Basic Engineering Package. Note that only one Sulfur Loading
Pump at a time is used for loading, regardless of whether one or both
loading spots are being used. Selector switch A2-HS15716 is used to
select which Sulfur Loading Pump is active.
(1) The truck driver spots his truck and connects the grounding
cable.
(4) The motive steam valve on the Sulfur Loading Vent Ejector at
that loading spot is opened and proven open.
(5) The sulfur loading valve at that loading spot is opened and
proven open.
If the other loading spot is not currently active, the "lead" pump
is started. If the other loading spot is active, the "lag" pump is
started. When selector switch A2-HS15716 is set to "NORMAL",
the "A" and "B" pumps will alternate in the "lead" position after
each loading operation. If A2-HS15716 is set to either "A" or "B",
only that pump is to be started even when both loading spots
are active.
(7) When its motor starter contacts show that the pump is running,
the discharge valve for that pump is opened and proven open.
(8) If the pump discharge valve is proven open before the timer on
that pump times out, the pump status light stops flashing and
remains steadily illuminated.
If the timer times out before the pump discharge valve is proven
open, the pump is stopped, its discharge valve is closed, its
status light is extinguished, and the corresponding "pump start
failure" alarm is activated.
(2) If the other loading spot is not currently active, stopping of the
"lead" pump is initiated. If the other loading spot is active,
stopping of the "lag" pump is initiated. The applicable pump
status light on the local loading control panel begins flashing.
(5) When its motor starter contacts show that the pump is stopped
and the limit switches show the pump discharge valve is closed,
the pump status light on the local loading control panel is
extinguished.
(6) The sulfur loading valve at that loading spot is closed and
proven closed.
(7) The motive steam valve on the Sulfur Loading Vent Ejector at
that loading spot is closed and proven closed.
(8) The discharge valve on the Sulfur Loading Vent Ejector at that
10.5.7.1 Causes
Any one of the devices listed below will activate the SDU ESD:
a. No Sulfur Feed Pump Running, A2-GA1532A&B and
A2-GA1542A&B starter contacts
10.5.7.2 Effects
A Sulfur Degassing Shutdown, activated by any one of the devices
listed above, has the following effects on the Sulfur Degassing Unit:
a. Shuts down the Sulfur Feed Pump, A2-GA1532A/B and
A2-GA1542A/B, to stop the flow of sulfur into the Sulfur
Degassing Reactor.
10.5.8.1 Causes
Any one of the causes listed below will activate the Sulfur Loading
ESD system:
a. Manual Shutdown Switches, A2-HS15727 and A2-HS15728
If neither the "lead" nor the "lag" Sulfur Loading Pump starts,
the Sulfur Loading ESD system is activated to shut down the
system and direct operator attention to the loading system.
10.5.8.2 Effects
For this reason, it is important that the degassing air not be introduced into
the Sulfur Degassing Reactor until it has been filled up to its normal
operating level with molten sulfur. This will ensure that if any iron sulfide
ever develops on the walls of the reactor, it will be immersed in the liquid
sulfur so that air cannot contact the walls directly and cause spontaneous
auto-ignition of the iron sulfide. The walls of the reactor above the normal
liquid level are always exposed to an oxygen-rich atmosphere, so iron
sulfide should not form above the air-liquid interface level in the reactor.
Note that the interior of the Sulfur Degassing Reactor is lined with a baked
phenolic coating to prevent iron sulfide from forming, but over time the
lining may deteriorate and expose some of the carbon steel.
When air first begins flowing through the Sulfur Degassing Reactor when
it is full of raw (not partially degassed) sulfur, it is possible for the H2S
concentration in the degassing air leaving the reactor to be above the
lower explosive limit for a short period of time if the air flow rate is too low.
For this reason, it is important to raise the air flow to its normal value
quickly when first starting air flow to the Sulfur Degassing Reactor with it
full of raw sulfur.
WARNING
CAUTION
After the initial startup, the Sulfur Storage & Loading system will also
contain sulfur throughout the system. Even when the sulfur is pumped out
of the Sulfur Storage Tank, the interior of the tank will still be coated with
residual sulfur. Elemental sulfur and/or iron sulfide in the Sulfur Storage
Tank may ignite when ventilating the tank with air prior to maintenance
operations. The heat from the fire can damage the tank if allowed to
continue burning, so use the snuffing steam to extinguish the fire should
this occur.
The walls of the tank above the liquid level are exposed to an oxygen-rich
atmosphere (due to the ventilation system sweeping air through the vapor
space of the tank), so little iron sulfide should form above the highest
air-liquid interface level in the tank. The middle region of the tank walls
should not have much iron sulfide, either, since the oxygen in the sweep
air will oxidize the iron sulfide as soon as the level is pumped back down.
However, the "heel" region of the tank may build up a considerable
quantity of iron sulfide, so auto-ignition of this iron sulfide is always a
potential problem when preparing the tank for maintenance.
Before the valve opens, the pressure in the vapor space of the Sulfur
Degassing Reactor should be at nearly atmospheric pressure, since
the spent degassing air is routed to the Thermal Oxidizer. The
degassing air line will also be at low pressure because the discharge
valve on the Degassing Air Blower will still be closed at this point,
even though the blower may be running. But when a Degassing Air
Blower is started and it's "reset" push-button is pressed, the PLC will
open the discharge valve on the blower. If there is back-pressure on
the Sulfur Degassing Reactor from the TTO when the discharge
valve opens, the pressure inside the Sulfur Degassing Reactor will
force liquid sulfur from the reactor up into the degassing air line. If
the back-pressure is high enough, liquid sulfur could overflow the
"loop seal" in the degassing air line, allowing sulfur to back down the
line to the Degassing Air Blower.
(3) Slowly "pinch" the blow-off valve until the discharge pressure
increases to 0.07-0.15 kg/cm2(g).
(5) Slowly close the blow-off valve the rest of the way to establish
air flow into the Sulfur Degassing Reactor.
(1) Confirm that the valve in its blow-off line is fully closed.
C. Start the off-line blower using its local start/stop control station.
Since its blow-off valve is still wide open at this point, the blower
will not be able to develop enough discharge pressure to open
the check valve in its discharge line.
E. Slowly "pinch" the blow-off valve on the off-line blower until its
discharge pressure rises enough to open its check valve and
begin sending some of its air to the Sulfur Degassing Reactor.
Observe the degassing air flow rate on the local indicator on the
degassing air flow transmitter and proceed slowly enough to
keep the degassing air flow rate stable.
H. Once the blow-off valve is fully closed on the one blower and
fully open on the other blower, the off-line blower is now the
on-line blower and vice versa. Use the local start/stop control
on what is now the off-line blower to stop that blower and close
its discharge valve, then close its blow-off valve.
Accordingly, the temperature inside the Sulfur Storage Tank and the
C. Check the rotation of the Degassing Air Blower and Sulfur Feed
Pumps:
E. Check all piping and equipment to be sure that all blinds have been
removed and that no valves are vented to atmosphere.
(1) Confirm that the steam supply valves to the steam coils in the
Sulfur Storage Tank are all closed, and that the steam trap
stations on each of the coils are all blocked-in.
(2) Establish steam flow into each of the coils by opening the
steam supply valves to each coil.
(3) Open the upstream block valve of the steam trap on each coil
and use the bleeder on each trap to vent air (and any liquids or
debris) from each coil. Close the bleeder on each trap once hot
condensate begins flowing through the trap.
(4) Open the test valve on each trap and confirm that each trap is
operating properly. Then close the test valve and open the
downstream block valve on each trap to place the traps in
service to the condensate header.
(6) Make sure that the breather vents at each quadrant of the top of
the Sulfur Storage Tank are unobstructed and that the air
sweep vent stack has begun to draft air into the tank through
the breather vents.
(7) Confirm that the block valve in the snuffing steam supply line for
the Sulfur Storage Tank is closed, and that the steam trap
station for the steam jackets on the snuffing steam shutdown
valve and the tank nozzle is blocked-in.
(8) Open the block valve in the snuffing steam supply line, then
open the upstream block valve of the steam trap and use its
bleeder to vent air (and any liquids or debris) from the piping
and jackets. Close the bleeder on the trap once hot
condensate begins flowing through the trap.
(9) Open the test valve on the trap and confirm that the trap is
operating properly. Then close the test valve and open the
downstream block valve to place the trap in service to the
condensate header.
(11) Confirm that the steam supply valves to the jacketed suction
and discharge piping on the Sulfur Loading Pump are all
closed, and that the steam trap stations on each pump's steam
jacket and the steam-jacketed piping are all blocked in.
(13) Establish steam flow into the jacketed piping and the steam
jackets on each pump by opening the steam supply valves.
(14) Allow air (and any liquids or debris) to purge from the vent
valves. Close each vent valve as it begins to blow steam.
(15) Open the upstream block valve of each steam trap on the
jacketed piping and the steam jackets on each pump, and use
the bleeder on each trap to drain water (and any other liquids)
from the pump and piping. Close the bleeder on each trap once
hot condensate begins flowing through the trap.
(16) Open the test valve on each trap and confirm that each trap is
operating properly. Then close the test valve and open the
downstream block valve on each trap to place the traps in
service to the condensate header.
(1) Confirm that the steam supply valves to the steam coils in the
Sulfur Surge Tank are all closed, and that the steam trap
stations on each of the coils are all blocked-in.
(2) Establish steam flow into each of the coils by opening the
steam supply valves to each coil.
(3) Open the upstream block valve of the steam trap on each coil
and use the bleeder on each trap to vent air (and any liquids or
debris) from each coil. Close the bleeder on each trap once hot
condensate begins flowing through the trap.
(4) Open the test valve on each trap and confirm that each trap is
operating properly. Then close the test valve and open the
downstream block valve on each trap to place the traps in
service to the condensate header.
(6) Make sure that the breather vents at the top of the Sulfur Surge
Tank are unobstructed and that the air sweep vent stack has
begun to draft air into the tank through the breather vents.
(7) Confirm that the ejector discharge valve is closed and the
ejector suction valve is open. Confirm that the motive steam
supply to the ejector is blocked-in. The ejector cannot be
placed in service until a TTO is operating.
(8) Confirm that the block valves in both of the snuffing steam
supply lines for the Sulfur Surge Tank are closed, and that the
(9) For each snuffing steam supply line, open the block valve in the
supply line, then open the upstream block valve of the steam
trap and use its bleeder to vent air (and any liquids or debris)
from the piping and jackets. Close the bleeder on the trap once
hot condensate begins flowing through the trap.
(10) Open the test valve on each trap and confirm that the traps are
operating properly. Then close the test valves and open the
downstream block valves to place the traps in service to the
condensate header.
(11) For each snuffing steam supply line, press the local push-button
to open the automated snuffing steam valve. Leave the valve
open long enough to confirm that steam is blowing into the tank,
then press the push-button again to close the valve. Visually
confirm that the valve has closed and that steam has stopped
flowing into the tank.
F. Establish steam flow into the jacketed pipe and the pumps by
opening the steam supply valve(s).
G. Allow air (and any liquids) to purge from the vent valves. Close each
vent valve as it begins to blow steam.
H. Open the upstream block valve of the steam trap on each pump and
use the bleeder on each trap to drain water (and any other liquids)
from each pump. Close the bleeder on each trap once hot
condensate begins flowing through the trap.
I. Open the test valve on each trap and confirm that each trap is
operating properly. Then close the test valve and open the
downstream block valve on each trap to place the traps in service to
the LP Condensate header.
(4) The bubbler tubes for all of the level transmitters in the two
Sulfur Surge Tanks and the Sulfur Storage Tank.
(5) The sulfur drain line, from the Sulfur Degassing Reactor, the
strainer, and the associated Degassed Sulfur Drain Seal
Assembly, A2-ME1550.
(7) The degassing air line feeding the Sulfur Degassing Reactor.
(8) The spent degassing air line from the Sulfur Degassing
Reactor.
Confirm that all steam traps are functioning properly before directing your
attention away from these heating systems.
WARNING
A. Place the Train 1 sulfur feed rate controller in the DCS in "manual"
and set its output to 0%.
B. Verify that the control valve in the associated Train 1 sulfur spill-back
line is fully closed.
C. Place Train 2 sulfur feed rate controller in the DCS in "manual" and
set its output to 0%.
D. Verify that the control valve in the Train 2 sulfur spill-back line is fully
closed.
E. Verify that the discharge valves on the Sulfur Feed Pumps for both
SRU trains are closed.
G. Open the block valve upstream of the strainer in the rundown line to
the Degassed Sulfur Drain Seal Assembly.
H. Confirm that the steam-out valve on the degassing air line is closed
and remove its blind flange.
K. When the oxygen concentration is below 1%, set the output of the
Train 1 sulfur feed rate controller to 100%
L. Verify that the control valve in the Train 1 spill-back line is fully open.
N. Close the block valve in the rundown line to the Degassed Sulfur
Drain Seal Assembly.
P. When the oxygen concentration is below 1%, open the block valve in
the spent degassing air line to the Thermal Oxidizer.
(1) Adjust the output of the Train 1 sulfur feed rate controller in the
DCS to 0% to close the spill-back valve.
(2) Remove the "forces" from the PLC and confirm that the
automated discharge block valves on the Train 1 Sulfur Feed
Pumps close.
R. Set the output of the Train 2 sulfur feed rate controller to 100%
S. Verify that the control valve in the Train 2 spill-back line is fully open.
U. Close the block valve in the spent degassing air line to the Thermal
Oxidizer.
W. When the oxygen concentration is below 1%, open the block valve in
the spent degassing air line to the Thermal Oxidizer.
(1) Adjust the output of the Train 2 sulfur feed rate controller in the
DCS to 0% to close the spill-back valve.
(2) Remove the "forces" from the PLC and confirm that the
automated discharge block valves on the Train 2 Sulfur Feed
Pumps close.
AA. Open the block valve in the rundown line to the Degassed Sulfur
Drain Seal Assembly.
BB. Close the block valve in the spent degassing air line to the Thermal
Oxidizer.
The Sulfur Degassing System is now ready for service. Once an SRU has
been started up and there has been sufficient sulfur production into a
Sulfur Surge Tank to commence operation of a Sulfur Feed Pump, sulfur
degassing can begin.
The following steps are based on placing the Train 1 Sulfur Feed Pump in
service first. The same procedures can be used for the Train 2 Sulfur
Feed Pump.
10.8.1.1 Filling the Sulfur Drain Seal in the Sulfur Outlet Line
CAUTION
D. Verify that the block valve in the sulfur rundown line, is open.
E. Verify that the shutdown valves in the discharge lines from the
Train 1 Sulfur Feed Pumps are closed.
G. The Train 1 sulfur flow meter should begin to indicate that sulfur
is flowing into the Sulfur Degassing Reactor.
H. It will take the Sulfur Feed Pump about 3-5 hours to fill the
Sulfur Degassing Reactor up to the top of the weir on the side
of its draw pan so that sulfur begins to flow out the degassed
sulfur outlet nozzle. Once it does so, it will take a few more
minutes for sulfur to fill the Degassed Sulfur Drain Seal
Assembly, A2-ME1550, and begin flowing into the Sulfur
Storage Tank. Open the view hatch on the Sulfur Drain Seal
and confirm that sulfur is now flowing into the tank.
WARNING
A. Confirm that the setpoint of the Train 1 sulfur feed rate flow
controller is tracking its current reading, then switch it to
"automatic" (not "cascade"). Slowly adjust the setpoint as
F. Confirm that the degassing air flow rate indicated in the DCS is
200 Nm3/H or higher.
G. Place the level controller for the Train 1 Sulfur Surge Tank in
service as follows:
(4) The setpoint of the level controller will be set at the last
reading. Adjust the setpoint to its normal value.
(2) Verify that the control valve in the Train 2 spill-back line is
closed.
(3) Verify that the shutdown valves in the discharge lines from
the Train 2 Sulfur Feed Pumps are closed.
(5) The Train 2 sulfur flow meter should begin to indicate that
sulfur is flowing to the Sulfur Degassing Reactor.
(6) Confirm that the setpoint of the Train 2 sulfur feed rate
flow controller is tracking its current reading, then switch it
to "automatic" (not "cascade"). Slowly adjust the setpoint
as necessary so that the spill-back valve opens to regulate
the sulfur feed rate to roughly the same value as the
current sulfur production rate.
(7) Place the level controller for the Train 2 Sulfur Surge Tank
in service.
(2) The level in the Train 1 Sulfur Surge Tank is under control.
(4) The level in the Train 2 Sulfur Surge Tank is under control.
(5) The degassing air flow rate is at its normal value or above.
2. Place all steam heating systems in service. Check all steam traps
for proper operation, and use the vent valves to sweep
non-condensibles out of the steam spaces.
The following steps are based on placing the Train 1 Sulfur Feed Pump in
service first. The same procedures can be used for the Train 2 Sulfur
Feed Pump.
CAUTION
D. Verify that the block valve in the sulfur rundown line is open.
E. Verify that the shutdown valves in the discharge lines from the
Train 1 Sulfur Feed Pumps are closed.
G. The Train 1 sulfur flow meter should begin to indicate that sulfur
is flowing into the Sulfur Degassing Reactor.
H. It will take the Sulfur Feed Pump about 3-5 hours to fill the
Sulfur Degassing Reactor up to the top of the weir on the side
of its draw pan so that sulfur begins to flow out the degassed
sulfur outlet nozzle. Once it does so, it will take a few more
minutes for sulfur to fill the Degassed Sulfur Drain Seal
Assembly, A2-ME1550, and begin flowing into the Sulfur
Storage Tank.
WARNING
A. Confirm that the setpoint of the Train 1 sulfur feed rate flow
controller is tracking its current reading, then switch it to
"automatic" (not "cascade"). Slowly adjust the setpoint as
necessary so that the spill-back valve opens to regulate the
sulfur feed rate to roughly the same value as the current sulfur
production rate.
E. Confirm that the degassing air flow rate indicated in the DCS is
200 Nm3/H or higher.
F. Place the level controller for the Train 1 Sulfur Surge Tank in
service as follows:
(4) The setpoint of the level controller will be set at the last
reading. Adjust the setpoint to its normal value.
(2) Verify that the control valve in the Train 2 spill-back line is
closed.
(3) Verify that the shutdown valves in the discharge lines from
the Train 2 Sulfur Feed Pumps are closed.
(5) The Train 2 sulfur flow meter should begin to indicate that
sulfur is flowing to the Sulfur Degassing Reactor.
(6) Confirm that the setpoint of the Train 2 sulfur feed rate
flow controller is tracking its current reading, then switch it
to "automatic" (not "cascade"). Slowly adjust the setpoint
as necessary so that the spill-back valve opens to regulate
the sulfur feed rate to roughly the same value as the
current sulfur production rate.
(7) Place the level controller for the Train 2 Sulfur Surge Tank
in service.
(2) The level in the Train 1 Sulfur Surge Tank is under control.
(4) The level in the Train 2 Sulfur Surge Tank is under control.
(5) The degassing air flow rate is at its normal value or above.
G. If sulfur does not begin flowing into the truck within 60 seconds, stop
the Sulfur Loading Pump by pressing the start/stop push-button. The
following items should be investigated to determine why sulfur is not
being pumped:
(1) Confirm that selector switch is set to the correct Sulfur Loading
Pump.
(2) Confirm that the "stop" switch for that pump, either is in the
"run" position.
I. Confirm that the Sulfur Loading Pump has stopped and its suction
and discharge valves are now closed.
CAUTION
D. If sulfur does not begin flowing into the truck within 60 seconds, stop
the Sulfur Loading Pump by pressing the start/stop push-button.
Investigate the items listed above to determine why sulfur is not
being pumped.
E. Once the sulfur truck is full, stop the sulfur loading operation by
pressing the start/stop push-button at the loading spot.
CAUTION
Typical shutdown procedures are outlined and discussed in the sections that
follow for the more common cases. Your existing company procedures and
common sense operational judgment should be used to modify these
procedures as needed to serve the purpose of any given planned shutdown
situation.
Stop the Sulfur Feed Pump, A2-GA1542A/B using its local start/stop
control push-button.
This should activate the SDU ESD system to shut down the
Degassing Air Blower.
B. Place the Train 1 sulfur feed rate controller in the DCS, in "manual"
and set its output to 0% to close the control valve in the spill-back
line.
Place the Train 2 sulfur feed rate controller in the DCS, in "manual"
and set its output to 0% to close the control valve in the spill-back
line.
This will prevent sulfur from draining out of the Sulfur Degassing
Reactor.
C. Visually confirm that:
(1) All Sulfur Feed Pumps are stopped, and that their discharge
valves are closed.
(2) Both Degassing Air Blowers are stopped and their discharge
valves are closed.
D. Confirm that all steam heating services are still functioning and the
steam traps are operating properly.
Stop the Sulfur Feed Pump, A2-GA1542A/B using its local start/stop
control push-button.
This should activate the SDU ESD system to shut down the
Degassing Air Blower.
B. Visually confirm that:
(1) All Sulfur Feed Pumps are stopped, and that their discharge
valves are closed.
(2) Both Degassing Air Blowers are stopped and their discharge
valves are closed.
C. Confirm that the block valve in the spent degassing air line is open to
the TTO.
Note: The sulfur from the Sulfur Degassing Reactor may be drained into
the surge tank for either SRU. Unless noted otherwise, the following
procedure applies to both Train 1 and Train 2.
D. Place the sulfur feed rate controller in the DCS, in "manual" and set
its output to 100%.
This will fully open the control valve in the spill-back line and allow all
of the liquid sulfur to empty from the Sulfur Degassing Reactor back
into the Sulfur Surge Tank.
E. Once the Sulfur Degassing Reactor is empty, set the output from the
flow controller to 0%.
Confirm that the control valve in the spill-back line is fully closed.
F. Remove the blind flange then open the steam-out valve on the
degassing air line and use LP steam to purge the gases in the Sulfur
Degassing Reactor out to the TTO.
I. Close the block valve in the sulfur drain line to isolate the Sulfur
Degassing Reactor from the drain trap and the Sulfur Storage Tank.
C. Briefly operate the other Sulfur Loading Pump until it loses suction to
remove as much sulfur as possible from the other suction sump.
D. Install slip blinds in the pump suction lines at the tank flanges.
E. Close the block valves in the steam and condensate lines for the
steam coils inside the tank, then de-pressure the coils.
F. Remove the covers from the roof and shell manholes, then use fans
or other means to sweep air through the tank and displace all of the
tank vapors.
G. If desired, the steam supply to the steam jacket on the air sweep
vent stack can be left in service so that the stack will help ventilate
the tank.
H. Monitor the air inside the tank and continue to sweep the tank with
air until no H2S is detected.
I. Once these steps have been completed, entry into the tank following
your company's policies for "confined space entry" should be
possible.
WARNING
Table of Contents
11. TAILGAS CLEANUP .............................................................................................. 11-1
11.1 PURPOSE OF SYSTEM ..................................................................................... 11-1
11.2 SAFETY ............................................................................................................... 11-2
11.3 PROCESS DESCRIPTION.................................................................................. 11-3
11.3.1 General ......................................................................................................... 11-3
11.3.2 Tailgas Hydrogenation/Hydrolysis ................................................................ 11-3
11.3.3 Process Gas Cooling .................................................................................... 11-4
11.3.4 Gas Contacting ............................................................................................. 11-5
11.3.5 Solvent Regeneration Section ...................................................................... 11-6
11.3.6 Steam Production/Consumption ................................................................... 11-7
11.4 EQUIPMENT DESCRIPTION .............................................................................. 11-8
11.4.1 TGCU Quench Column, A2-DA1560 ............................................................ 11-8
11.4.2 TGCU Quench Column Packing, A2-DB1560 .............................................. 11-8
11.4.3 TGCU Contactor, A2-DA1561 ...................................................................... 11-8
11.4.4 TGCU Contactor Packing & Internals, A2-DB1561 ...................................... 11-8
11.4.5 TGCU Stripper, A2-DA1562 ......................................................................... 11-9
11.4.6 TGCU Stripper Trays, A2-DB1562 ............................................................... 11-9
11.4.7 TGCU Reactor, A2-DC1560 ....................................................................... 11-10
11.4.8 TGCU Stripper Reflux Accumulator, A2-FA1560 ....................................... 11-10
11.4.9 Catalyst for TGCU Reactor, A2-MC1560 ................................................... 11-10
11.4.10 TGCU Stripper Reboiler Condensate Pot, A2-FA1562 ........................... 11-10
11.4.11 TGCU Reactor Feed Heater, A2-EA1560 ............................................... 11-11
11.4.12 TGCU Waste Heat Reclaimer, A2-EA1561 ............................................ 11-11
11.4.13 TGCU Quench Water Trim Cooler, A2-EA1562A/B ................................ 11-11
11.4.14 TGCU Lean/Rich Exchanger, A2-EA1564 .............................................. 11-11
11.4.15 TGCU Stripper Reboiler, A2-EA1565 ..................................................... 11-12
11.4.16 TGCU Lean Amine Trim Cooler, A2-EA1563 ......................................... 11-12
11.4.17 TGCU Quench Water Cooler, A2-EC1560 ............................................. 11-12
11.4.18 TGCU Stripper Reflux Condenser, A2-EC1562 ...................................... 11-12
11.4.19 TGCU Lean Amine Cooler, A2-EC1561 ................................................. 11-12
11.4.20 TGCU Quench Water Pump, A2-GA1560A/B......................................... 11-13
11.4.21 TGCU Rich Amine Pump, A2-GA1561A/B ............................................. 11-14
11.4.22 TGCU Stripper Reflux Pump, A2-GA1563A/B ........................................ 11-14
11.4.23 TGCU Lean Amine Pump, A2-GA1562A/B ............................................. 11-14
11.4.24 TGCU Start-Up Blower, A2-GB1560 ....................................................... 11-14
11.4.25 Refractory for TGCU Reactor, A2-MR1560 ............................................ 11-15
11.4.26 TGCU Reactor Feed Mixer, A2-ME1560 ................................................ 11-16
11.7.5 Leak Testing the Process Piping and Equipment ....................................... 11-75
11.7.6 Washing the Quench Water System .......................................................... 11-79
11.7.6.1 Water Flush ......................................................................................... 11-79
11.7.6.2 Acid Wash ........................................................................................... 11-82
11.7.6.3 Alkaline Wash...................................................................................... 11-82
11.7.6.4 Initial Water Fill .................................................................................... 11-84
11.7.7 Washing the Amine System ....................................................................... 11-85
11.7.7.1 Water Flush ......................................................................................... 11-86
11.7.7.2 Acid Wash ........................................................................................... 11-89
11.7.7.3 Weak Amine Wash .............................................................................. 11-91
11.7.7.4 Initial Solvent Fill ................................................................................. 11-93
11.7.8 Purging the Low Pressure TGCU Columns ................................................ 11-97
11.7.8.1 Establishing Nitrogen Flow .................................................................. 11-97
11.7.8.2 Purging the TGCU Start-Up Blower .................................................... 11-99
11.7.8.3 Purging the Columns ......................................................................... 11-100
11.8 STARTUP PROCEDURES.............................................................................. 11-102
11.8.1 Initial Startup of the TGCU ....................................................................... 11-102
11.8.1.1 Initial Preparations............................................................................. 11-102
11.8.1.2 Establishing Nitrogen Flow ................................................................ 11-103
11.8.1.3 Establishing Re-circulation Flow ....................................................... 11-104
11.8.2 Pre-Sulfiding the TGCU Catalyst .............................................................. 11-107
11.8.2.1 Establishing Reducing Gas Flow....................................................... 11-108
11.8.2.2 Pre-Sulfiding the Catalyst .................................................................. 11-111
11.8.3 Routing SRU Tailgas to the TGCU ........................................................... 11-115
11.8.3.1 Introducing SRU Tailgas into the TGCU — Scenario 1 ..................... 11-116
11.8.3.2 Introducing SRU Tailgas into the TGCU — Scenario 2 ..................... 11-119
11.8.4 Quench Water and Amine Systems ......................................................... 11-122
11.8.5 Process Gas Flow to the TGCU Columns ................................................ 11-124
11.8.6 Normal Startup of the TGCU .................................................................... 11-128
11.8.6.1 Initial Preparations............................................................................. 11-128
11.8.6.2 Purging the Low Pressure TGCU Columns....................................... 11-130
11.8.6.3 Establishing Nitrogen Flow ................................................................ 11-130
11.8.6.4 Establishing Re-circulation Flow ....................................................... 11-131
11.8.6.5 Establishing Reducing Gas Flow....................................................... 11-133
11.8.6.6 Routing SRU Tailgas to the TGCU.................................................... 11-134
11.8.6.7 Quench Water and Amine Systems .................................................. 11-138
11.8.6.8 Process Gas Flow to the TGCU Columns ......................................... 11-140
11.9 SHUTDOWN PROCEDURES ......................................................................... 11-144
11.9.1 Planned Shutdown - No Reactor Entry..................................................... 11-145
11.9.2 Planned Shutdown for Reactor Entry ....................................................... 11-151
11.9.3 Shutting Down When Boiler Tubes Are Leaking ...................................... 11-158
11.9.4 Special Precaution During Shutdowns ..................................................... 11-159
11.9.5 Emergency Shutdown .............................................................................. 11-163
11.9.6 Effects of Shutdowns and Outages in Other Systems.............................. 11-164
11.9.6.1 Amine Regeneration Unit Outages.................................................... 11-164
11.9.6.2 Sour Water Stripper Outages ............................................................ 11-164
11.9.6.3 Sulfur Recovery Unit ESD System .................................................... 11-164
11.9.6.4 Thermal Oxidizer ESD System.......................................................... 11-165
11.9.6.5 Steam System Outage ...................................................................... 11-166
11.10 ANALYTICAL PROCEDURES ..................................................................... 11-167
11.10.1 General Procedures for Analyzing TGCU Solvent, ............................... 11-167
11.10.2 Determination of Amine Concentration in TGCU Solvent ..................... 11-171
11.10.3 Determination of Total Acid Gas Loading in TGCU Solvent ................. 11-173
11.10.4 Determination of H2S and CO2 Loading in TGCU Solvent .................... 11-175
11.10.5 Determination of Foaming Tendency of TGCU Solvent ........................ 11-179
11.10.6 H2S Conc. in TGCU Contactor Ovhd by the Tutweiler Method ............. 11-181
11.10.7 H2S Conc. in TGCU Contactor Ovhd Using Gas Detector Tubes ......... 11-182
11.10.7.1 Operating Principles.......................................................................... 11-182
11.10.7.2 Sampling the TGCU Contactor Overhead Gas ................................. 11-183
11.10.7.3 Calculations ...................................................................................... 11-184
11.10.8 Monitoring the Performance Level of TGCU Catalyst ........................... 11-185
Treated vent gas from the Tailgas Cleanup Unit (TGCU) is routed to the Tailgas
Thermal Oxidation system and afterwards dispersed to the atmosphere. Due to
the sulfur removal by the TGCU process, the incinerated effluent gas will
normally contain less than 200 PPMV of SO2 on a dry, 0% oxygen basis.
11.2 Safety
WARNING
The Tailgas Cleanup Unit (TGCU) receives tailgas from the two Sulfur
Recovery Units and uses the Shell Claus Off-gas Treating (SCOT)
process licensed by Shell Global Solutions (US) Inc. for sulfur removal.
The TGCU Unit has been designed to process the 7,655 Nm3/H of sulfur
plant tailgas that results when each SRU receives a total fresh acid gas
feed containing 34.6 MT/D of sulfur. The TGCU process reduces all of the
sulfur compounds in the sulfur plant tailgas to H2S, then uses selective
amine absorption to recover H2S from the tailgas while allowing most of
the CO2 to "slip" by. The H2S and CO2 removed by the amine are stripped
from the amine and recycled to the two SRUs, allowing an overall sulfur
recovery in excess of 99.9 wt. %.
Less than 220 PPMV of sulfur (wet basis, expressed as H2S) remains in
the treated effluent flowing to the Tailgas Thermal Oxidation Unit. This
sulfur content is low enough to keep the SO2 content of the incinerated
effluent below 200 PPMV (on a dry, 0% oxygen basis) when the H2S and
sulfur in the spent degassing air from the Sulfur Degassing Unit and the
sweep air from the Sulfur Surge Tanks are included, due to the dilution
effect of the thermal incineration process.
(2) S + H2 H2S
Carbon monoxide in the tailgas also reacts with the water vapor in the gas
to form hydrogen, the classic "water gas shift" reaction:
The partially cooled gas from the TGCU Waste Heat Reclaimer enters the
bottom of the TGCU Quench Column, A2-DA1560, for the second stage of
cooling. As the gas passes upward through the packed bed in this tower,
it is further cooled by direct contact with a circulating stream of quench
water. As the gas is cooled, most of the water vapor produced by the
upstream reactions (Claus, combustion, and hydrogenation) is condensed
and removed from the gas stream. In addition to cooling the gas, direct
contact with the quench water serves to absorb trace quantities of SO2
that may "break through" the TGCU Reactor periodically. Since SO2 will
react with amines to form heat-stable salts, the "washing" action of the
quench water helps minimize degradation of the MDEA solvent.
The cooled gas stream leaves the top of the TGCU Quench Column at
39°C [102°F] and flows to the TGCU Contactor, A2-DA1561, while the
quench water exits the bottom of the tower at 67°C [153°F]. The TGCU
Quench Water Pump, A2-GA1560A/B, circulates the water stream to the
TGCU Quench Water Cooler, A2-EC1560, and the TGCU Quench Water
Trim Cooler, A2-EA1562A/B, to reject the heat removed in the TGCU
Quench Column. This cools the quench water to 38°C [104°F] before it is
returned to the top of the tower.
A sidestream of the quench water flows through the TGCU Quench Water
Filter, A2-FD1560A/B, to remove solids from the quench water system. A
portion of the filtrate is routed to the Sour Water Stripping Unit to balance
the water condensed from the gas in the TGCU Quench Column, on level
control from the tower. The remainder of the filtrate returns to the suction
of the circulating pump.
The reactions between the acidic gases and the basic amine solution can
be represented by:
The selectivity of the solvent for H2S over CO2 is important since the
absorbed gases are recycled to the SRUs. Minimizing CO2 pickup
reduces the amount of gas recycling to the sulfur plants, and allows the
equipment in the Sulfur Recovery and Tailgas Cleanup Units to be
smaller.
The selectivity of tertiary amines like MDEA for H2S is a result of the
indirect reaction that must occur between the amine and CO2. Unlike
The rich amine leaves the bottom of the tower at 42°C [108°F] and is
pumped by the TGCU Rich Amine Pump, A2-GA1561A/B, through the
TGCU Rich Amine Filter, A2-FD1562A/B, to remove accumulated solids.
The rich amine then flows on level control through the tube side of the
TGCU Lean/Rich Exchanger, A2-EA1564A/B/C, and is preheated to
105°C [221°F] by cooling the lean amine before flowing to the TGCU
Stripper, A2-DA1562, entering between trays #4 and #5.
Gaskets are installed where the bed support and distributor tray bolt to the
support ring and clips inside the TGCU Quench Column to prevent direct
contact between the stainless steel internals and the carbon steel vessel.
This electrically isolates the dissimilar metals from each other to prevent
direct contact that could lead to galvanic corrosion.
Gaskets are installed where the bed support and distributor tray bolt to the
support ring and clips inside the TGCU Quench Column to prevent direct
contact between the stainless steel internals and the carbon steel vessel.
This electrically isolates the dissimilar metals from each other to prevent
direct contact that could lead to galvanic corrosion.
A chimney tray is located below the bottom valve tray to gather all of the
column liquids to feed the TGCU Stripper Reboiler. The column section
located below this chimney tray serves to separate the outlet steam and
lean amine from the reboiler and to provide surge for the solvent
circulating system.
The chimney tray gathers the tower liquids to feed the reboiler. The outlet
from the reboiler reenters the column below the chimney tray, with the
vapor produced by the reboiler flowing upward through the chimneys in
order to reach the valve trays above.
The top four trays in the column are located above the rich amine feed
point and serve as water-wash trays to minimize the amount of amine
carried-over in the tower overhead. Since these trays have only the reflux
water flowing over them, the liquid rates for these trays are much lower
than for the trays lower in the column. For this reason, these four trays
are designed for minimum leakage (i.e., picket fence weirs, minimum
downcomer clearance, etc.).
As stated above, this vessel is simply a very good steam trap. During
normal operation, the steam pressure required to provide the necessary
reboil heat to the TGCU Stripper may be much less than the
3.5-4.2 kg/cm2(g) steam pressure available in the LP steam system. The
normal steam pressure in the shell of the reboiler may be such that the
water level in the condensate pot will rise upwards from the pot, perhaps
even within the shell of the reboiler. During these periods, the level valve
will remain fully open and the sight glass will indicate a full water level.
This is a normal operating condition for this vessel. The vessel will usually
operate with a visible level only when the TGCU Stripper Reboiler is
operating near its maximum capacity with full steam pressure on the shell
of the exchanger. Under these conditions, the level control and level
valve will function normally and maintain a water level in the vessel.
The boiler is equipped with level transmittersthat will shut down the TGCU
should the water level fall to within 75 mm of the top row of tubes.
Operation of the boiler without a sufficient water level could possibly
damage the tubes.
CAUTION
WARNING
THE LIQUID IN THESE PUMPS CONTAINS DISSOLVED H2S. THIS H2S CAN
BE RELEASED TO THE SURROUNDINGS WHEN LIQUID IS DRAINED FROM
THESE PUMPS OR FROM THE PIPING CONNECTED TO THE PUMPS.
ALWAYS OBSERVE PROPER PROCEDURES AND PRECAUTIONS WHEN
DRAINING LIQUID FROM THESE PUMPS OR PERFORMING MAINTENANCE
ON THEM. THE "GENERAL SAFETY" SECTION OF THESE GUIDELINES
SHOULD BE CONSULTED IF THERE IS ANY DOUBT ABOUT HOW TO WORK
SAFELY WHEN H2S MAY BE PRESENT.
The blower casing and impeller are constructed of carbon steel and
coated with "Heresite", a baked phenolic coating, for corrosion resistance.
WARNING
CAUTION
WARNING
WARNING
Thus, here are two important control parameters: the reactor feed
temperature and the hydrogen concentration in the reactor feed. The loop
diagram on page 11-22 illustrates the components of these control loops
when implemented in a distributed control system (DCS).
There are also controls for handling specific requirements during startup
and shutdown of the front-end of the TGCU. These control loops are
shown on the loop diagram as well. All of the control loops are discussed
in the sections that follow.
match the increase in the heat input. The net result is to increase the
heat transfer, raising the feed temperature accordingly.
The process gas that is being sampled is saturated with water, so the
data sheet for the analyzer system specifies that the sample
conditioning system includes a dryer. For the sample point on the
outlet of the TGCU Waste Heat Reclaimer, there is also the
possibility of elemental sulfur vapor being present in the gas during
process upsets. To prevent sulfur from reaching the analyzer and
damaging it, a "sacrificial sample loop" consisting of a coil of bare
tubing is provided in this sample line. The tubing coils provide heat
transfer surface, so that if sulfur does find its way to this point in the
process, the gas will cool off enough for the sulfur to solidify,
plugging the sample loop and stopping the flow of process gas to the
analyzer before the sulfur can damage the analyzer. Should this
occur, only the coiled tubing will need to be replaced, rather than the
expensive analyzer. Note that the sample lines are to free-drain from
the analyzer back to the sample points, so the tubing coils should be
oriented in the horizontal so that the coils due not cause a "pocket" in
the sample line for this sample point.
b. Prior to the initial startup of the unit, the catalyst in the TGCU
Reactor must be pre-sulfided so that it retains its activity when it
c. After the TGCU has been operating for a period of time, the
catalyst becomes pyrophoric due to the presence of iron sulfide,
FeS. Exposing catalyst containing pyrophoric FeS to air may
result in uncontrolled burning of the FeS to form H2S and/or
SO2, which obviously will prevent the entrance of personnel into
the vessel. When the TGCU is to be shut down to replace the
catalyst, or for other maintenance activities that will allow
oxygen to enter the reactor, it is necessary to perform a
controlled oxidation ("passivation") of the FeS in the catalyst by
operating at low temperature (~150°C [~300°F]) and controlling
a small concentration (1-2%) of oxygen in the circulating gas.
This converts the FeS into non-pyrophoric iron oxide, Fe2O3,
while leaving the catalyst in its sulfided state. Flow controller
A2-FIC15805 is provided to allow adding a small amount of
utility air to the nitrogen circulating through the front-end of the
unit to provide the oxygen for catalyst passivation.
The H2/H2S analyzer can sample the process gas from two different
locations, depending on the position of the selector valve inside the
analyzer enclosure. The first sample connection is on the outlet of the
TGCU Waste Heat Reclaimer. It should be used only during startup,
pre-sulfiding, and other special operations when the process gas is
bypassing the quench and contacting sections. This connection has a
"sacrificial" sample line, which is essentially a disposable sample cooling
coil. It is intended to protect the analyzer by cooling, condensing, and
freezing any sulfur vapor that may be present in the sample due to
process upsets. If this occurs, the cooling coil will plug before the sulfur
can reach the analyzer, sacrificing the inexpensive tubing to protect the
expensive analyzer.
The second sample point is on the overhead line from the TGCU
Contactor, and is the normal sampling point. During startup of the TGCU,
the hydrogen analyzer should be switched to this sample point as soon as
the Quench Column hand control in the DCS is used to open the Quench
Column Inlet Valve and close Quench Column Bypass Valve to send gas
through the TGCU Quench Column and the TGCU Contactor. There is
much less chance of damaging the analyzer with contaminants when
sampling gas at this point, so it is the preferred sample connection.
CAUTION
(3) After being notified to proceed by the DCS operator, the outside
operator blocks-in A2-LT15845A by closing its block valves,
then opens the drain valve on the bottom of the transmitter to
drain the water from the instrument.
(4) If the transmitter is operating properly, the DCS will alarm that
there is a low level in the Waste Heat Reclaimer on
A2-LI15845A. The DCS operator acknowledges the alarm on
the DCS and reports it to the outside operator.
(5) After being notified of the alarm, the outside operator closes the
drain valve on A2-LT15845A, slowly opens its bottom block
valve to allow the transmitter to fill with water then opens its top
block valve. This should clear the low level alarm on
A2-LI15845A in the DCS.
(6) After confirming that the low level alarm has cleared, the other
level transmitters can be tested in a similar fashion.
NOTE: The DCS operator must not begin another task until confirming
that the low level alarm has cleared. This is to guard against
having a level transmitter malfunction that causes a TGCU ESD
when the other transmitters are tested.
For this reason, the TGCU ESD is an input to the PLC interlock
blocks that manipulate the controllers (A2-HIC15457, A2-HIC15462,
A2-HIC15657, and A2-HIC15662) for these valves. The PLCs and
DCS automatically reposition the valves following a TGCU ESD to
divert the SRU tailgas to the TTO, meaning that the valves are
already positioned properly for the subsequent restart of the TGCU.
The logic that accomplishes this for the Train 1 SRU is depicted on
the logic flow diagram. When the TGCU ESD is activated, the
Train 1 SRU PLC directs the DCS to set the output from
A2-HIC15457 to 100% to open A2-HV15457, proves the valve open,
then directs the DCS to set the output from A2-HIC15462 to 0% to
close A2-HV15462 and proves the valve closed. This diverts the
Train 1 SRU tailgas directly to the TTO. (The PLC logic will not take
these actions if the Train 1 SRU has its startup/run selector switch,
A2-HS15314, set to "STARTUP", since both tailgas valves will already
be closed by the startup logic for the Train 1 SRU)
Note that this same logic is also used to open the tailgas valve to the
TTO and close the tailgas valve to the TGCU if the TGCU startup/run
selector switch (A2-HS15830) is set to "STARTUP". This safeguard is
to prevent sending SRU tailgas into the TGCU before the TGCU
Reactor is ready, as this could cause a severe upset in the TGCU
Quench Column and/or TGCU Contactor (and possibly damage the
piping, equipment, quench water, and/or solvent).
2. The PLC directs the DCS to set the output from A2-HIC15462 to
100% to open the Tailgas Valve to the TGCU, A2-HV15462, then
proves that the valve is open.
7. Once one or both of the tailgas valves to the TGCU is open and
the corresponding tailgas valve(s) to the TTO are closed, the
operator can use A2-HIC15800 in the DCS to close
A2-NV15800.
8. This will force all of the SRU tailgas to flow to the TGCU Reactor
Feed Heater.
10. All of the SRU tailgas will now be flowing through the TGCU
Reactor Feed Heater, TGCU Reactor Feed Mixer, TGCU
Reactor, and TGCU Waste Heat Reclaimer, then flowing to the
TTO via the TGCU Quench Column bypass valve, A2-HV15851,
at the TGCU Startup Blower. Once the plant stabilizes and there
is excess hydrogen in the reactor outlet, the TGCU Quench
Column inlet valve, A2-HV15850, can be opened and
A2-HV15851 closed using A2-HIC15850 in the DCS to send the
process gas into the TGCU Quench Column and TGCU
Contactor.
and block it from flowing into the TGCU. Once the problem has been
corrected, A2-HS15463 and A2-HS15663 can be toggled once again
to "TRANSFER TO TGCU" to send the SRU tailgas into the TGCU.
(3) If the SRUs and TGCU did manage to stay on-line, the TGCU
Reactor Feed Heater would be supplying less than half as
much heating as needed until the controls recover and bring the
steam flow rate up to the new requirements.
So, the best that could be expected if the second SRU is routed to
the TGCU in the same manner as under the first scenario is an upset
in both SRUs, the TGCU Reactor Feed Heater, the TGCU Reactor,
the quench water system, and the solvent system. Depending on
how quickly the SRUs respond to sudden changes in operating
pressure, the SRU burners might flame-out. In this worst case, a
complete restart of the SRUs and the TGCU would then be required.
Instead of introducing the tailgas from the second SRU into the
TGCU in an abrupt manner, what is needed is a slow, controlled
redirection of the tailgas from the TTO to the TGCU. This can be
accomplished by the DCS operator using A2-HIC15457 and
A2-HIC15462:
2. The DCS operator initiates the over-ride for the Train 1 tailgas
valves by toggling the "slow" transfer switch, A2-HS15464 in the
DCS, to "OVER-RIDE".
11.5.5.1 Causes
Any one of the causes listed below will activate the TGCU ESD
system:
11.5.5.2 Effects
A TGCU shutdown, activated either manually or automatically, has
the following effects on the TGCU:
c. Disables the "fast" and "slow" tailgas transfer switches for the
Train 1 SRU (A2-HS15463 and A2-HS15464, respectively) and
for the Train 2 SRU (A2-HS15663 and A2-HS15664,
respectively).
d. Shuts off and depressurizes the nitrogen and plant air supplies
by closing block valves A2-NV15809 and A2-NV15811 and
opening vent valve A2-NV15810.
Do not use water to quickly cool the TGCU Reactor after a fire. Not only
will this damage the catalyst, the rapid cooling may cause structural
damage to the TGCU Reactor. The acidic water that forms may cause
corrosion damage to the TGCU Reactor or other equipment. Nitrogen is
available to the TGCU for use in cooling a hot catalyst bed.
CAUTION
(2) S + H2 H2S
The catalyst also promotes the classic "water gas shift" reaction:
This effectively converts carbon monoxide in the tailgas gas into hydrogen
for use in reactions (1) and (2) above. This is an equilibrium reaction, so it
is typical for a small amount of CO to leave a reactor, depending on the
amount of hydrogen and carbon dioxide in the reactor outlet. The CO
concentration in the reactor outlet is usually less than 100 PPM, but may
be higher if the CO2 content of the feed gas is high or if the catalyst has
lost activity.
NOTE: A small portion of the COS and CS2 may either not react at all,
or be reduced by the hydrogen to form methane and/or methyl
mercaptan:
All of these reactions are exothermic, causing the temperature of the gas
to rise as it flows through the reactor. The hydrogenation of the SO2 into
H2S is the predominant factor in the temperature rise, so the temperature
rise across the TGCU Reactor is usually a direct indication of the amount
of SO2 entering the TGCU from the SRUs. If the temperature rise is
higher than normal (about 50-60°C at design conditions), this is usually a
sign that the upstream sulfur plant(s) is off-ratio. The resulting high outlet
temperature from the TGCU Reactor cannot be corrected in the TGCU.
Rather, the problem must be corrected in the SRUs, or the upstream units
feeding the SRUs.
Regardless of the amount of SO2, sulfur vapor, and organic sulfur entering
the TGCU Reactor, all of it must be converted to H2S for proper operation
of the downstream equipment. This can be achieved (assuming normal
catalyst activity) by maintaining an adequate excess of hydrogen in the
TGCU Reactor outlet, so that all of the reactions go to completion. The
hydrogen concentration is normally measured in the treated gas leaving
the TGCU Contactor. Although the design material balance calls for a
hydrogen concentration of about 3% at this point, a concentration in the
range of 1-2% is normally adequate. However, controlling the
concentration at 3% or higher allows a much larger margin for tolerating
upsets in the upstream SRUs, and is generally preferred.
Unlike other TGCUs which use in-line burners to generate reducing gas
(because external hydrogen is not available), this TGCU receives
reducing gas from a hydrogen purification unit. However, poor ratio control
in either SRU can still lead to an excessively high outlet temperature from
the TGCU Reactor. If, for instance, an SRU is operating with excess air,
the H2S:SO2 ratio will be low in the SRU tailgas (registered as high air
demand) and the SO2 concentration will be high in the TGCU Reactor
feed. This will cause a large temperature rise in the reactor. Left
unchecked, the temperatures in the TGCU Reactor could rise to the point
of damaging the catalyst, the catalyst bed support, and/or the reactor
vessel itself. The thermocouples in the catalyst bed and in the outlet line
have alarms to provide an early warning of this condition. If the
temperature reaches 400°C in the outlet line, the TGCU ESD system will
be activated to shut down the TGCU and divert the SRU tailgas to the
Thermal Oxidizer, before damaging the TGCU Reactor or its catalyst.
Be aware, however, that the "thermal mass" of the TGCU Reactor and its
catalyst bed is quite large relative to the gas flowing through them, so
temperature changes occur very slowly (particularly at low flow rates). For
this reason, it is important to watch the temperature trends around the
reactor and be prepared to take corrective action early so that the
corrections have time to take effect before a high-high temperature
shutdown is activated. It is particularly important to watch these
temperatures closely during periods of startup, shutdown, or
process upsets when the TGCU Reactor inlet temperature,
composition, and/or flow rate are changing significantly.
The quench water circulation rate is controlled by the quench water flow
controller in the DCS, while the temperature is controlled by a temperature
controller adjusting the speed of one of the fans on the TGCU Quench
Water Cooler, A2-EC1560. Although the design values will give adequate
operation, there are advantages in maintaining the quench water
temperature (which controls the overhead temperature) as low as
possible. These conditions will minimize the temperature and water
content of the overhead gas leaving the TGCU Quench Column and thus
minimize the load on the TGCU Contactor. The bottoms temperature of
the TGCU Quench Column is not critical except for controlling corrosion;
this temperature depends on the gas feed rate and the temperature and
flow rate of the circulating quench water. However, operating the quench
water at a lower or higher temperature than the TGCU lean amine can
cause the TGCU amine system to be out of water balance. Normally,
both the quench water and the TGCU amine should operate at roughly the
same temperature to minimize the impact on the amine system water
balance.
A portion of the quench water is sent to SWS Flash Drum on level control
to balance the water condensed from the process gas by the circulating
quench water and maintain the bottoms level in the TGCU Quench
Column. This "bleed" water rate depends on the amount of water in the
SRU tailgas, and the amount of water contained in the gas leaving the
column.
The TGCU Quench Water Filter removes sulfur and particulates from the
circulating quench water to maintain water clarity. The flow rate to the
filter should be maintained at its design value to provide maximum
filtration.
If sufficient acid is formed to drop the pH of the quench water below 7, the
acid will often scour the iron sulfide film (which normally protects the steel
from corrosion) from the carbon steel equipment and piping. The iron
sulfide particles will turn the quench water black (or green). Either color
change (milky or black/green) is a symptom of SO2 "break-through" from
the TGCU Reactor, meaning that inadequate reducing gas is being
supplied to the reactor. An abnormal increase in the pressure drop across
the TGCU Quench Water Filter is also a good indication of SO2
break-through, as the sulfur and/or iron sulfide particles collect on the filter
elements.
If a large SO2 deviation occurs (very low pH, very dirty quench water,
rapid plugging of the TGCU Quench Water Filter, etc.), it may be desirable
to dilute the quench water with fresh condensate makeup. This
accomplishes two things to facilitate cleanup of the quench water system:
the fresh makeup will dilute the SO2 and help raise the pH, and the
makeup will raise the level in the TGCU Quench Column and cause the
quench water column level controller to increase the "bleed" rate of
quench water to the Sour Water Stripping Unit. The rate at which
condensate is added to the system must be regulated to keep the
temperature to the circulating pump low enough that the pump does not
cavitate. Experience will show how quickly condensate can be added
without causing pumping problems.
In addition, consider diverting the process gas from the TGCU Reactor to
the Thermal Oxidizer before it enters the TGCU Quench Column during
periods of large upsets when SO2 may break through the reactor, before
SO2 gets into the quench water and causes problems. Taking this
preventative measure will cause higher SO2 emissions from the Thermal
Oxidizer and put it out of compliance, but it will allow the TGCU to be
brought back to normal operation much more quickly by avoiding a pH
excursion in the quench system and the water cleanup operation that
often results (i.e., numerous filter changes in the TGCU Quench Water
Filter).
The TGCU Reactor effluent will then be diverted to the Thermal Oxidizer
and cannot cause problems in the TGCU columns if SO2 escapes from
the reactor. Once the upset has been corrected and gas flow into the
columns can be re-initiated by increasing the output on the Quench
Column bypass hand controller in the DCS to 100% output to restore flow
to the columns. These changes should be performed slowly enough to
minimize the "bobbles" on the air:acid gas ratio control in the SRUs, as
the operating pressures in the units will change as the valves are
The important parameters for controlling the H2S content of the TGCU
Contactor vent gas, assuming the amine is adequately stripped, are amine
temperature, amine flow rate, and contact time. The design values for
amine temperature and flow rate shown on the Process Flow Diagram
should give satisfactory operation, but it is possible to adjust these values
either to maximize the capacity of the system to tolerate upsets, or to
optimize the "slipping" of CO2 to the vent gas. The following discussion
should be helpful if improving plant operations is desired.
The amine strength should be monitored and the amine content of the
circulating amine should be maintained close to the 45% (by weight)
design value. Should the amine concentration decrease (normally due to
blowdown and other amine losses), it will be necessary to add fresh amine
to compensate. Laboratory procedures for analyzing TGCU amine are
given in Section 11.10 of these guidelines.
(3) A2-HV15457 The Tailgas Valve to the TTO can leak SRU
A2-HV15657 tailgas directly to the Thermal Oxidizer.
Check the SO2 emissions after stroking each valve. If the emissions are
still high after checking all the valves, then verify that both the H2S
analyzer and the SO2 analyzer are calibrated properly. If these valves are
not leaking, there is usually no obvious reason why these two analyzers
should show a discrepancy in the sulfur content of the TGCU effluent.
CAUTION
The withdrawal of lean amine from the bottom of the TGCU Stripper is on
flow control to the TGCU Contactor. As a result, the level in the bottom of
the TGCU Stripper, which serves as the "surge" for the system, will
usually indicate if adjustments of water makeup to the amine system (or
water "bleed" from the system) are required to maintain the proper water
balance. Even if water must be bled from the system by diverting some of
the column reflux to The SWS Flash Drum, the amine content of that
waste stream should be low and only infrequent makeup of fresh amine
should be required.
There is full-flow of rich amine through the TGCU Rich Amine Filter, and a
slipstream of lean amine flow through the TGCU Lean Amine Filter, the
TGCU Amine Carbon Filter, and the TGCU Amine After-Filter. These four
filters will remove solids and organic contaminants from the circulating
amine, such as degradation or corrosion products. The flow rate through
the lean amine filters should be maintained at the design value, and the
filter elements should be changed as soon as the "change" pressure drop
is reached, to remove as many solids from the amine as possible. Finely
divided solids can cause foaming and thereby limit column capacity.
While it is possible to reduce foaming to some extent with anti-foam
agents, the presence of such agents may also reduce H2S/CO2 selectivity
in the TGCU Contactor, so it is preferable that they not be used as an
alternative to regular conscientious filter maintenance
A. The water content of the feed gas to the TGCU Contactor (the
overhead from the TGCU Quench Column).
B. The water content of the vent gas leaving the TGCU Contactor.
C. The water content of the TGCU recycle gas leaving the TGCU
Stripper Reflux Accumulator.
D. The amount of water makeup to (or water "bleed" from) the amine
system.
For given operating pressures, the water content of each gas stream will
be determined by the temperature at the top of the respective vessel
(TGCU Quench Column, TGCU Contactor, and TGCU Stripper Reflux
Accumulator, respectively), and will increase as the temperature
increases. Since the TGCU Contactor inlet gas is at a slightly higher
pressure than the outlet (vent) gas, the inlet gas will normally contain less
water than is contained in the outlet gas (if both gas streams are at the
same temperature), thus requiring water makeup to maintain the proper
water content of the amine. This situation will be reversed if the TGCU
Contactor overhead temperature is lower than the TGCU Quench Column
overhead temperature, requiring a "bleed" of water to maintain water
balance.
Since the lean amine to the TGCU Contactor is on flow control and
withdrawal of the rich amine from the bottom of the TGCU Contactor is on
level control, a net gain or loss in the amine water balance will be reflected
by an increase or decrease, respectively, of the liquid level in the bottom
of the TGCU Stripper. Observation of this liquid level can thus guide
adjustment of water makeup/bleed rate or operating conditions to maintain
the desired water concentration of the circulating amine. Since the degree
of H2S removal can depend on the amine concentration of the amine, the
concentration should be maintained close to the design value (45 wt %)
by appropriate maintenance of water concentration. It is usually possible
to control the water balance without adding fresh water or "bleeding" water
to the Sour Water Stripping Unit by adjusting the operating temperatures
in the unit, as discussed in the following paragraphs. Following the steps
outlined below will allow controlling the water balance with minimum
usage of treated makeup water and minimum impact on the sour water
system.
(2) Begin "bleeding" water (or increase the "bleed" water rate) from
the amine system with the flow controller on the discharge line
of the TGCU Stripper Reflux Pump.
CAUTION
This will increase the amount of water leaving in the vent gas,
but it will also reduce the H2S-removal capability of the solvent.
An increase in solvent flow rate will probably be needed to
maintain the same H2S content in the vent gas, increasing the
load on the TGCU Stripper and the other process equipment
associated with the circulating solvent. Additionally, some
impairment of the CO2 "slip" by the solvent would be expected
as a result of both the higher contact temperatures in the TGCU
Contactor and the higher solvent circulation. This will increase
the CO2 recycled to the sulfur plants and increase the CO2
content of the tailgas to the TGCU, further hampering the
H2S-removal capability of the solvent.
Although this will increase the water content of this stream and
reduce the water in the solvent, the effect will be small because
the quantity of recycle gas is small relative to the vent gas, and
the pressure of the recycle gas is considerably higher. This
adjustment is the least effective and would not normally be
considered during routine operations.
4. Begin water makeup (or increase the makeup water rate) to the
solvent system using the make-up flow controller to add
condensate to the TGCU Stripper Reflux Accumulator. The
TGCU Stripper Reflux Pump will then send the makeup water to
the TGCU Stripper, increasing the water content of the TGCU
solvent.
This will increase the water content of the gas entering the
TGCU Contactor, but it also increases the vapor load and
hampers H2S removal, so this step should not be taken to
extremes.
Amine degradation can occur via reaction with SO2, which can enter the
TGCU Contactor during periods when insufficient reducing gas is fed to
the TGCU Reactor. During such periods, most of the SO2 "breaking
through" the TGCU Reactor should be scrubbed out in the TGCU Quench
Column. However, any traces of SO2 entering the TGCU Contactor will
react with the MDEA to form a thermally non-regenerable complex (i.e.,
heat-stable salt). If present in sufficient quantity, this salt can alter the
H2S-amine equilibrium and prevent removal of H2S to the desired level in
the TGCU Contactor overhead. Heat-stable salts also increase the
corrosivity of the TGCU amine. Amine quality can be restored by
treatment with an amount of caustic equivalent to the non-regenerable salt
present but, if repeated caustic treatments are necessary due to repeated
mal-operation, the potential for salt deposition in the system may rise.
The equipment in the TGCU, including the seals of pumps and blowers,
should be operated at positive pressure to minimize the potential for
oxygen (air) ingress into the amine. Oxygen will react with the amine to
produce carboxylic acids that cause the solution to be corrosive. For this
same reason, it is important to maintain an inert gas "blanket" on the
MDEA storage tank to prevent oxygen contamination of the fresh amine.
Amine losses due to entrainment in the vent gas or the recycle gas can be
minimized by proper process operation (avoidance of column overloading,
foaming, etc.) and routine inspection of the vessel internals. Amine losses
in the water "bleed" from the TGCU Stripper reflux should be negligible if
the rectifying trays (the "wash water" trays above the amine feed point) in
the TGCU Stripper are operating properly (no flooding or foaming, no
mechanical damage).
The primary source of amine loss will likely be the mechanical losses from
pump drips, cleaning of filters, etc. Good housekeeping practices,
including prompt replacement or repair of leaking pumps, together with
proper collection of amine drips for reuse will minimize the mechanical
loss of amine.
The TGCU contains three columns: the TGCU Quench Column and the
TGCU Contactor, which contain structured packing; and the TGCU
Stripper, which contains valve trays. In general, the liquid feed rate to
packed towers can decrease in proportion with the gas flow rate down to
about 50% of design gas flow rate. Below this point, the liquid rate cannot
be allowed to drop any further without risking poor column performance
due to uneven liquid distribution and wetting of the packing. Trayed
towers typically offer somewhat better turndown, allowing the liquid rate to
drop to 30-40% of design before "weeping" of the trays begins to
significantly affect performance.
At a total acid gas feed rate of 14 MT/D (of contained sulfur) to the SRUs,
the gas flow rates to the TGCU Quench Column and the TGCU Contactor
will be about 40% of design. In the case of the TGCU Quench Column,
simply setting the quench water flow rate to the column at about 50% of
design should maintain adequate performance. (It should be noted,
however, that there is really no detrimental effect if the quench water
circulation is simply left at the design value at all times. The only
drawback is slightly higher power consumption by the pump and aerial
cooler.)
In the packed TGCU Contactor, circulating more amine relative to the gas
flow rate should maintain performance. The liquid flow rate should be
maintained at a minimum of about 50%.
This higher amine circulation also has the advantage of absorbing more
CO2 from the TGCU Contactor feed, which is subsequently stripped from
the amine and recycled back to the SRUs. While TGCUs are normally
operated to minimize CO2 pickup, increasing the CO2 pickup in this
situation is advantageous. It raises the mass flow rate in the SRUs and
the TGCU, minimizing the operating problems throughout the SRU/TGCU
systems by preventing sulfur fog formation in the Sulfur Condensers. A
higher circulation rate also means the TGCU has more capacity to remove
H2S from the amine, making it less likely that SRU upsets will cause SO2
emissions to exceed permit limits. It will also keep the TGCU Stripper
trays well above their minimum operating rate.
The first step in identifying the cause of the high pressure drop is to
determine which equipment pass or section of piping contains the
restriction. (It is unusual to have more than one area of high pressure
drop.) This is best accomplished by making a pressure survey of the
process side of the TGCU (and the SRUs and Thermal Oxidizer, if
necessary).
Due to the low operating pressure in the TGCU (generally 0.3 kg/cm2(g) or
less) and the low pressure drop in each equipment pass (generally
0.00-0.04 kg/cm2 per pass), a single pressure gauge must be used to
make the pressure survey in order to get meaningful results. The gauge
should be a low pressure gauge for best results (a -1 - 0 - +1.5 kg/cm2
gauge is recommended).
Beginning at the front end of the TGCU, use the pressure tap valves on
the inlet and outlet lines from each equipment pass to measure the
pressure at each point in the process. Proceed toward the back end of
the process until the pass with the high pressure drop is found. Note that
some of the pressure tap valves may be plugged with solid sulfur.
Rod-out the sample valves as necessary to obtain an accurate pressure
reading.
WARNING
There are many qualified boiler and water treatment companies that can
advise the owner/operator on chemical treatment testing and controls. It
is recommend that only those companies that have local technicians with
extensive experience specifically in boiler water treatment be selected to
assist with Samsung Total Petrochemicals Co., Ltd.'s program.
The design details incorporated in the TGCU Waste Heat Reclaimer have
proven to be very reliable when combined with good operator practice
regarding water treatment. However, even properly designed equipment
can be severely damaged during a short period of operation if the water
treatment program is inadequate or improper.
Prior to using the intermittent blowdown valve, use the level controller in
the DCS to raise the water level in the boiler up to the high level alarm
point. Then open the intermittent blowdown valve until the level drops
back to the normal liquid level. Watch the boiler level in the sight glass
throughout this operation to ensure that the level is not lost (which would
activate the TGCU ESD and shut the TGCU down). Remember to reset
the level controller at the conclusion of this procedure.
D. Check the rotation of the fans on the TGCU Quench Water Cooler,
the TGCU Lean Amine Cooler, and the TGCU Stripper Reflux
Condenser, by operating each fan for a short period.
E. Check all piping and equipment to be sure that all blinds have been
removed and that no valves are vented to atmosphere.
B. Use the quick-opening blowdown valve to lower the water level in the
boiler and check for proper operation of the level transmitters, the
low level alarms, and the low-low level shutdowns.
C. Fill the boiler with treated boiler feed water back up to the normal
liquid level.
F. Check all relief valves to ensure that they are installed in the proper
locations and set for the correct relieving pressures.
G. The low-low level shutdowns for the pumps in the quench water and
amine systems will be tested while washing these systems as
described in the following sections.
A. Place the utility air controller in the DCS in "manual" and set its
output to 0%.
B. Place the nitrogen controller in the DCS in "manual" and set its
output to 0%.
C. Confirm that the following nitrogen and utility air valves are closed:
(1) The upstream block valve, flow control valve, and the
downstream block valve in the nitrogen supply line.
(2) The upstream block valve, flow control valve, and the
downstream block valve in the utility air supply line.
(4) The block valve in the HP nitrogen supply line located near the
TGCU Reactor.
(5) The gate valves upstream and the ball valves downstream of
the flow indicators in the purges to the sensing lines for the
TGCU Reactor d/P transmitter.
(6) The ball valves in the sensing lines for the TGCU Reactor d/P
transmitter.
(7) The gate and ball valves in the purge line to the shaft seal on
the TGCU Start-Up Blower.
(8) The gate valve in the LP nitrogen supply line, and the ball valve
downstream of the flow indicator in the purge line to the TGCU
Start-Up Blower discharge line.
(9) The gate valve upstream of the flow indicator in the supply line
to the sample switching valve for the H2/H2S analyzer.
(10) The block valves in the nitrogen supply line to the TGCU
Stripper Reflux Accumulator.
D. Confirm that all of the manual vent/drain valves in the nitrogen and
utility air piping are closed.
E. If the orifice plate has already been installed in the utility air flow
meter, remove it for now
F. If the orifice plate has already been installed in the nitrogen flow
meter, remove it for now
G. Disconnect the nitrogen and utility air from the tailgas line by
performing the following steps:
(3) Cover the open end of the piping to prevent debris from
entering when the upstream piping is blown down.
H. Confirm that the H.P. nitrogen, L.P. nitrogen, and Utility Air supply
headers have been placed in service, with the pressure regulators
set properly and the safety relief valves in service, and with the main
supply header piping blown down and drained.
I. Rotate the spectacle blind in the utility air line to the "open" position.
K. "Force" the PLC to open the two nitrogen blocks, and close the
nitrogen vent valve.
M. "Crack" the upstream block valve in the main utility air supply line
and allow air to blow through the piping until it is clear. Then close
the block valve, reinstall the utility air supply pressure regulator, and
reopen the block valve.
N. Using the utility air supply pressure regulator and the vent valve
downstream of the pressure control valve, adjust the utility air
regulator to the setpoint specified on the P&IDs.
O. "Crack" the block valve in the main nitrogen supply line and allow
nitrogen to blow through the piping until it is clear. Then close the
gate valve, reinstall the nitrogen supply pressure regulator, and
reopen the gate valve.
P. Using the pressure gauge and the vent valve downstream of the
nitrogen supply pressure regulator, adjust the nitrogen regulator to its
specified setpoint.
Q. Open the flow valve in the utility air line by setting the output of the
flow controller to 100% in the DCS, then use the downstream drain
valve to blow out this section of piping. Close the drain valve when
the piping is clear.
R. Open the flow valve in the nitrogen line by setting the output of the
flow controller to 100% in the DCS, then use the downstream drain
valve to blow out this section of piping. Close the drain valve when
the piping is clear.
S. "Crack" the block valve downstream of the flow valve and allow air to
blow through the piping until it is clear. Then close the bock valve.
T. Close the flow valve in the utility air line by setting the output of the
flow controller to 0% in the DCS
V. Close the control valve in the nitrogen line by setting the output of the
flow controller to 0% in the DCS
W. Remove the "forces" from the PLC and confirm that both of the
automated block valves close and the automated vent valve opens.
X. Close the upstream block valve in the utility air supply line.
Y. Rotate the spectacle blind in the utility air line to the "closed"
position.
Z. Close the upstream block valve in the nitrogen supply line until the
TGCU unit is ready for startup.
AA. Reconnect the nitrogen / air piping by performing the following steps:
(1) Reinstall the steam jacketed block valve and bolt the flanged
connections back together.
(4) Reinstall the orifice plate in the utility air flow meter.
BB. Open the block valve in the utility nitrogen supply line located near
the TGCU Reactor until the line is clear.
CC. The TGCU Reactor d/P transmitter has low pressure purges for both
of its sensing lines, each with a rotameter near where it connects to
the sensing line. Disconnect the upstream fitting at each rotameter
and briefly open its upstream gate valve to blow any liquids or debris
from its purge line. Reconnect each rotameter, disconnect the fitting
where each purge connects to the sensing line, open the upstream
gate valve, and open the ball valve downstream of each rotameter
briefly to blow any liquids or debris from the purge lines. Then
reconnect each purge to the sensing line and open its valve to place
it in service.
DD. Disconnect the fitting where each sensing line connects to its
process line, and open the ball valve in each sensing line briefly to
blow any liquids or debris from the lines. Then reconnect each
sensing line to its process line and open its ball valve to place it in
service.
NOTE: The two rotameters must be adjusted to the same flow rate
so that the pressure drop of the purge gas in the sensing
lines does not affect the reading of the d/P transmitter. One
EE. Disconnect the upstream fitting (in the purge line to the shaft seal on
the TGCU Start-Up Blower) and open the upstream gate and ball
valves briefly to blow any liquids or debris from the purge line.
Reconnect the rotameter and disconnect the fitting where the purge
connects to the shaft seal. Open the upstream gate valve, open the
ball valve briefly to blow any liquids or debris from the purge line,
then reconnect the purge to the shaft seal and open the ball valve to
place it in service.
FF. The nitrogen purge valve for the blower casing should already be
open. Disconnect the upstream fitting (in the purge line to the TGCU
Start-Up Blower discharge line) and open the upstream gate valve
briefly to blow any liquids or debris from the purge line. Reconnect
the rotameter and disconnect the fitting where the purge connects to
the discharge line on the TGCU Start-Up Blower. Open the
upstream gate valve, open the downstream ball valve briefly to blow
any liquids or debris from the purge line, then reconnect the purge to
the discharge line.
GG. Re-open the ball valve downstream of the nitrogen purge valve and
allow the nitrogen to pressurize the TGCU Start-Up Blower and the
piping inside the suction and discharge block valves. Check all of
the blower and piping connections for visible or audible signs of
leakage (by applying masking tape or "Snoop" to the flanges,
listening for other leaks, etc.). When done, leave the ball valve open
so that the purge is in service.
HH. Disconnect the upstream fitting (in the nitrogen supply line to the
sample switching valves) and open the upstream gate valve briefly to
blow any liquids or debris from the purge line. Reconnect the
rotameter and disconnect the fitting where the purge connects to the
sample selector valve on the H2/H2S analyzer. "Crack" the gate
valve to blow nitrogen through the piping until it is clear. Then close
the gate valve, reconnect the piping, and reopen the gate valve.
JJ. "Crack" the upstream block valve in the nitrogen supply line and
allow nitrogen to blow through the piping until it is clear. Then close
the block valve, reinstall the nitrogen supply pressure regulator, and
reopen the block valve.
KK. Using the nitrogen supply pressure regulator and the vent valve
downstream of the regulator, adjust the nitrogen regulator to the
setpoint specified on the P&IDs
A. Place the hydrogen controller in the DCS in "manual" and set its
output to 0%.
(2) The reducing gas supply line automated block valves, the flow
control valve, the isolation valve downstream of the control
valve and the bypass valve around the control valve.
D. If the orifice plate has already been installed in the hydrogen flow
meter, remove it for now.
E. Rotate the spectacle blind in the hydrogen supply line to the "closed"
position.
F. Disconnect the hydrogen piping from the line going to the TGCU
Reactor Feed Mixer by performing the following steps:
(3) Cover the open end of the piping to prevent debris from
entering when the upstream piping is blown down.
H. "Force" the PLC to open the block valves in the hydrogen supply line,
and close the vent valve.
K. "Crack" the gate valve upstream of the pressure regulator and allow
nitrogen to blow through the piping until it is clear. Then close the
gate valve, reinstall the pressure regulator and reopen the gate
valve.
L. Using the pressure gauge and the vent valve downstream of the
pressure regulator, adjust the hydrogen regulator to the setpoint
specified on the P&IDs.
M. Open the reducing gas supply line control valve by setting the output
of the hydrogen controller to 100% in the DCS, then use the
downstream drain valve to blow out this section of piping. Close the
drain valve when the piping is clear.
N. "Crack" the gate valve downstream of the reducing gas supply line
control valve and allow nitrogen to blow through the piping until it is
clear. Then close the gate valve.
O. Close the reducing gas supply line control valve by setting the output
of the hydrogen controller to 0% in the DCS.
P. Briefly open the bypass valve around the control valve and allow
nitrogen to blow through the piping until it is clean. Then close the
bypass valve.
Q. Remove the "forces" from the PLC and confirm that both of the
automated block valves close and the automated vent valve opens.
(1) Reinstall the steam jacketed block valve and bolt the flanged
connections back together.
(5) Rotate the spectacle blind in the hydrogen supply line to the
"open" position.
(1) Open the two gate valves upstream of the pressure regulator.
(2) "Crack" the bypass valve to vent hydrogen to the flare. Adjust
the pressure regulator if necessary to maintain its setpoint,
observing the pressure on the pressure gauge.
(3) Close the bypass valve, and the gate valve immediately
upstream of the pressure regulator.
CAUTION
The process piping and equipment in the TGCU can be checked for leaks
by using nitrogen to pressurize the process side of the equipment and
piping to about 0.6-0.7 kg/cm2(g), then checking flanges, etc. for leaks
(usually by applying masking tape or "Snoop" to the flanges, and by
listening for other leaks). In order to pressurize the TGCU with nitrogen, it
is necessary to block-in the unit by closing the outlet valve. This
procedure requires some special preparations to operate in this manner,
as detailed below.
This same procedure can be used to leak test the TGCU following
maintenance, before restarting the unit. Whenever plant maintenance
requires opening one or more of the flanged connections in the TGCU, it
is good practice to leak test the unit before returning it to service. This
allows detecting any leaking connections that may have resulted from the
maintenance operations before tailgas is reintroduced into the unit.
B. Confirm that the Quench Column inlet hand control in the DCS is set
to 0% output so that the TGCU Quench Column Bypass Valve will
open later in Step F when the Startup/Run selector switch is
switched to "STARTUP".
C. Confirm that the TGCU Quench Column is isolated from the quench
water circulation loop by confirming that the following valves are all
closed:
(1) The bypass valve and downstream block valve at the quench
water flow control valve.
(5) The block valve in the caustic supply line at the tie-in to the
suction line.
(6) The block valve in the condensate fill line at the tie-in to the
suction line.
(7) The bypass valve and downstream block valve at the filtered
quench water flow control valve.
(1) The bypass valve and downstream block valve at the lean
solvent flow control valve.
(4) The block valves in the solvent makeup line at the tie-in to the
suction line.
(5) The block valve and globe valve in the condensate makeup line
at the tie-in to the suction line.
E. Confirm that the spectacle blind in the utility air supply line is in the
"closed" position.
G. Confirm that the SRU Tailgas Valves to the TGCU are closed.
H. Confirm that the TGCU Start-Up Blower Bypass Valve is fully open.
I. Confirm that the block valve(s), and the steam-jacketed block valve
in the nitrogen supply line are open.
(1) Bypasses the TGCU ESD to allow opening the nitrogen supply
valves via the nitrogen on/off push-button.
M. Use the nitrogen flow controller in the DCS to open the nitrogen flow
control valve and send nitrogen to the TGCU to begin pressurizing it.
N. Slowly increase the output from the nitrogen flow controller until the
pressure reaches 0.6-0.7 kg/cm2(g) as measured by the pressure
indicator in the DCS.
Due to the volume inside the TGCU, it will take several minutes for
the pressure to build up in the unit.
O. Once the desired pressure has been achieved, set the output from
the nitrogen flow controller to 0% to close the nitrogen flow control
valve. Check all of the equipment and piping connections for visible
or audible signs of leakage.
The PLC will enable all of the ESDs for the TGCU again.
Failure to clean the system properly prior to startup can lead to operating
problems (heat exchanger fouling, rapid filter plugging, etc.).
WARNING
C. Confirm that the Quench Column inlet hand control in the DCS
is set to 0% output so that the TGCU Quench Column inlet
valve is fully closed.
E. Verify that the quench water flow control valve is fully open.
Open both of its isolation block valves and its bypass valve.
F. Verify that the TGCU Quench Column level control valve is fully
closed. Close both of its isolation block valves and its bypass
valve.
G. Verify that the TGCU Quench Column inlet valve is fully closed.
(This will prevent water from entering the TGCU Reactor if the
TGCU Quench Column is accidentally over-filled.)
H. Verify that the filtered quench water flow control valve is fully
open. Open both of its isolation block valves and its bypass
valve.
I. The TGCU Quench Water Filter will not be used to filter solids
during this time, but the filter vessel and its piping are to be
flushed and cleaned. Remove the filter elements, then bolt-up
the filter. Open the inlet and outlet block valves on the filter,
and open the bypass valve around the filter.
O. Watch the level in the TGCU Quench Column while placing the
pump in service to be sure the pump does not lose suction
while filling the downstream piping and equipment. If the level
Q. Use the low point drain valves to flush out each section of the
system. Leave the drain valves open until the water is clear.
S. Circulate the water and blow down the low point drains until all
of the drain water is clear. Add more condensate as necessary
to maintain the level in the TGCU Quench Column.
U. Allow the pump to continue running while the system drains, but
watch the pump closely to verify that the low-low level shutdown
shuts the pump down below the shutdown setpoint. If the level
drops completely out of the gauge glass before the pump shuts
down, stop the pump manually and correct the problem with the
low-low level shutdown before proceeding further.
V. Verify that the caustic supply line has been flushed and is ready
for service.
G. After 6 hours, shut down the pump and completely drain the
system. Drain the system as quickly as possible, so that the
liquid velocity will help flush any remaining solids from the
system.
D. Allow the pump to run for long enough to displace the water in
the caustic supply piping (left from the earlier water flush
procedure). Add caustic to the circulating water to make a
0.02 wt% solution. This should give a pH in the range of 11-22.
E. Shut off the TGCU Caustic Injection Pump, and close the block
valve in the caustic supply at the injection point in the quench
water piping.
G. After circulating for about 1 hour, start the other TGCU Quench
Water Pump and shut down the first one.
J. After 2 hours, shut down the pump and completely drain the
system. Drain the system as quickly as possible, so that the
liquid velocity will help flush any remaining solids from the
system.
A. Close the inlet and outlet block valves on the TGCU Quench
Water Filter, then install the proper element(s) in the filter.
Leave the block valves closed for now.
(2) "Crack" the filter inlet block valve open slightly and allow
the filter to fill with water. When the filter is full, close the
vent valve.
(3) Open the filter inlet block valve fully and open the outlet
block valve, then close the filter bypass valve.
(4) Place the filtered quench water flow controller in the DCS
in service and set its setpoint to its normal value. Close
I. Allow the pump to run for a few minutes until the pH of the
solution is in the range of 12-13.
J. Shut off the TGCU Caustic Injection Pump and close its suction
valve. Leave the block valve at the injection point in the quench
water piping open.
The quench water system is now ready for service. It can remain in
this operating mode indefinitely while the rest of the TGCU is
prepared for startup. Check the system periodically for indications of
plugging, etc. (low flow, erratic pump discharge pressure, high filter
pressure drop), as solid materials may accumulate at various points
in the system over time.
Failure to clean the system properly prior to startup can lead to operating
problems (column foaming, poor treating, heat exchanger fouling, rapid
filter plugging, etc.).
WARNING
(a) Set the output from the lean solvent flow controller to 100% to
fully open the lean solvent flow control valve.
(b) Open the manual block valve upstream of the lean solvent
filters.
(c) Set the output from the TGCU Contactor level controller to
100% to fully open the TGCU Contactor level control valve.
(d) Set the output from the TGCU Stripper Reboiler steam
flow controller to 0% to fully close the steam flow control valve.
(f) Set the output from the bleed water flow controller to 0%
to fully close the bleed water flow control valve.
(g) Set the output from the makeup water flow controller to
0% to fully close the makeup water flow control valve.
(3) The TGCU Contactor level control, (the rich solvent from
the TGCU Contactor).
D. Verify that the following control valves are fully closed. Close
both of the isolation block valves and the bypass valve at each
control station.
(3) The bleed water flow control valve from the TGCU Stripper
reflux.
(4) The makeup water flow control valve to the TGCU Stripper
Reflux Accumulator.
E. Verify that the bypass valve on the pressure control valve to the
flare is closed. Open both of the isolation block valves at this
control station.
F. The TGCU solvent filters will not be used to filter solids during
this time, but the filter vessels and their piping are to be flushed
and cleaned. Remove the filter elements, then bolt-up the
individual filters. Open the inlet and outlet block valves on each
filter, and open the bypass valves for the filters.
G. Verify that the valves in the solvent makeup line are closed.
Watch the level in the TGCU Contactor as the pump fills the
downstream piping and begins to fill the TGCU Stripper. When
the level drops to the low-low level shutdown should shut down
the pump. If it does not, stop the pump manually before it loses
suction and correct the problem with the low level shutdown
before proceeding.
N. At this point, neither the flow into or the level of the TGCU
Contactor is being controlled. Both control stations are in
"manual" with the valves fully open to flush the piping as much
as possible. Depending on the hydraulics of the system, it may
be necessary to place either or both of these controls in
"automatic" to prevent losing the level in one of the columns. If
so, leave the bypass valve on the control station "cracked" so
that the bypass piping gets flushed.
O. Use the low point drain valves to flush out each section of the
system. Leave the drain valves open until the water is clear.
P. Circulate the water and blow down the low point drains until all
of the drain water is clear. Add more condensate as necessary
to maintain the levels in the columns.
Q. Once the drain water is clear, shut down the TGCU Rich Amine
Pump and completely drain the system. Drain the system as
quickly as possible, so that the water velocity will help flush the
solids from all parts of the system.
S. Confirm that the solvent transfer line (for MDEA makeup) has
been flushed and is ready for service.
D. It is unlikely that any steam will leave the top of the TGCU
Stripper during this operation, so the TGCU Stripper Reflux
Accumulator should remain dry. If a level should develop in this
vessel, drain the water from the vessel using a drain valve on
one of the TGCU Stripper Reflux Pumps.
E. After circulating for about 3 hours, start the other TGCU Rich
Amine Pump and shut down the first one. Do the same with the
TGCU Lean Amine Pumps.
G. After 6 hours, shut off the steam to the TGCU Stripper Reboiler,
shut down the pumps, and completely drain the system. Drain
the system as quickly as possible, so that the liquid velocity will
help flush any remaining solids from the system.
I. Switch to the other pumps for a few minutes, then shut down
the pumps and completely drain the system.
P. Once the reflux loop has cleared up (the drain water is clear),
shut off the steam to the TGCU Stripper Reboiler, shut down
the pumps, and completely drain the system. Drain the system
as quickly as possible, so that the liquid velocity will help flush
any remaining solids from the system.
G. During one of the pumping cycles for the TGCU Stripper Reflux
Accumulator, flush out the minimum flow spill-back line by
opening the manual block valve to allow circulation through this
line. Then close the manual block valve.
H. During another pumping cycle, flush out the bleed water piping
by setting the output of the bleed water flow controller to 100%
to fully open the bleed water flow control valve, opening its
upstream and downstream block valves, and opening its
bypass valve. Then close the valves and set the output of the
bleed water flow control valve back to 0%.
J. Once the solution drained from all the low point drain valves is
clear, shut off the steam to the TGCU Stripper Reboiler, shut
down the pumps, and completely drain the system. Drain the
system as quickly as possible, so that the liquid velocity will
help flush any remaining solids from the system.
L. Switch to the other pumps for a few minutes, then shut down
the pumps and completely drain the system.
A. Close the inlet and outlet block valves on the four TGCU
solvent filters, then install the proper elements and/or carbon in
the filters. Leave the block valves closed on each filter for now.
F. Open the high point vent valve on the TGCU Stripper overhead
line and allow the steam to purge any air from the vessel. As
the pressure builds, the vent valve can be closed.
H. Ensure that the fans are running on the TGCU Lean Amine
Cooler and the TGCU Stripper Condenser. Commence cooling
water flow to the TGCU Lean Amine Trim Cooler.
L. If the control loops on the TGCU solvent have not already been
placed in service, do so at this time. Switch the TGCU
contactor level controller and the lean solvent flow controller in
the DCS to "automatic" with their setpoints set to their normal
values.
(2) "Crack" the filter inlet block valve open slightly and allow
the filter to fill with solvent. When the filter is full, close its
vent valve.
(3) Open the inlet and outlet block valves on the filter.
(4) Slowly close the valve in the bypass line around the filter.
O. Flush the makeup water line by setting the output from the
makeup water flow controller to 100% to fully open the makeup
water flow control valve, opening its upstream block valve, then
opening the downstream drain valve until the water runs clear.
Then set the output of the flow controller to 0% to close the
makeup water flow control valve, and open the downstream
block valve.
The solvent system is now ready for service. It can remain in this
operating mode indefinitely while the rest of the TGCU is prepared
for startup. Check the system periodically for indications of plugging,
etc. (low flow, erratic pump discharge pressure, high filter pressure
drop), as solid materials may accumulate at various points in the
system over time.
2. The quench water system and perhaps the amine system have
been cleaned and loaded with their respective initial fills of water
and amine. (The amine system may be waiting on purging of the
TGCU Contactor before the system is loaded with amine.)
B. Confirm that the Quench Column inlet hand control in the DCS
is set to 0% output so that the TGCU Quench Column Bypass
Valve will open later in Step F when the Startup/Run selector
switch is switched to "STARTUP".
(5) The block valve in the caustic supply line at the tie-in to
the suction line.
(6) The block valve in the condensate fill line at the tie-in to
the suction line.
(1) The bypass valve and downstream block valve at the lean
solvent flow control valve.
(4) The block valves in the solvent makeup line at the tie-in to
the suction line.
E. Confirm that the spectacle blind in the utility air supply line is in
the "closed" position.
G. Confirm that the SRU Tailgas Valves to the TGCU are closed.
L. Set the output of the hand control in the DCS to 0% to close the
TGCU Warmup/Bypass Valve.
N. Use the nitrogen flow controller in the DCS to open the nitrogen
flow control valve and send nitrogen to the front end of the
TGCU.
(4) After the limit switches prove these valves open, the
TGCU Start-Up Blower is started.
Reactor Feed Heater and TGCU Reactor Feed Mixer and all of
the associated piping.
(2) Prove the bypass valve open using the limit switches.
A. Open all of the vent valves on the PI and PDT taps on the
TGCU Quench Column and the TGCU Contactor, and the vent
valves at the tops of the columns.
B. Increase the output from the Quench Column inlet hand control
in the DCS to 100% to open the TGCU Quench Column Inlet
Valve and close the TGCU Quench Column Bypass Valve.
NOTE: If the initial solvent fill was not loaded into the solvent
system earlier to avoid exposing the MDEA to oxygen, this
can be accomplished now. Follow the procedure given in
the previous section to fill the solvent system with its initial
solvent charge.
J. Confirm that the Quench Column hand control in the DCS is set
to 0% output, so that the TGCU Quench Column inlet valve will
remain fully closed and the TGCU Quench Column bypass
valve will open later when the TGCU startup/run selector switch
is switched to "STARTUP".
Q. Verify that the local stop control for the TGCU Start-Up Blower
is set to the run position.
(4) After the limit switches prove these valves open, the
TGCU Start-Up Blower is started.
G. Confirm that the BFW level controller and control valve to the
TGCU Waste Heat Reclaimer are in service and functioning
properly.
(1) Confirm that the remote setpoint that the reactor feed
temperature controller is supplying to the pressure
controller matches the current setting on the pressure
controller.
Also, ensure that there is an adequate supply on hand (one or two boxes)
of gas detector tubes for measuring the H2S concentration into and out of
the TGCU Reactor. Sections 9.10.8 and 11.10.7 of these guidelines
describe how Dräger tubes can be used to measure the H2S
concentration of a gas stream. The H2S concentration will probably be in
the range of 1-2%, so Dräger Catalog No. CH 281 01 gas detector tubes
are appropriate.
(2) Disconnect the sample line from the sample valve and
from the 2-way analyzer sample switching valve. Drain any
water from the line and check that it is not plugged, then
reinstall the sample line.
(3) Repeat Step (2) for the other sample line (connected to
the sample valve on the TGCU Contactor overhead line).
CAUTION
Look for signs that the H2S has begun to react with the catalyst
(i.e. the temperatures in the reactor begin to rise). If no
CAUTION
If any of these conditions are not true, do not attempt to bring SRU tailgas
into the TGCU. In particular, do not attempt switching tailgas into the
TGCU when the SRU(s) is(are) experiencing an upset. The result will
be multiple upset units to deal with. Instead, focus your attention on
stabilizing the operation of the SRU(s) first (usually by correcting a
problem in the upstream Amine Regeneration and/or Sour Water Stripper
units), and then use the procedure that follows to establish tailgas flow
into the TGCU.
(2) After the limit switches prove this valve open, the SRU 1
Tailgas Valve to the TTO is closed.
At this point, the tailgas from SRU 1 can flow to the TTO via either of
two routes:
(1) Through the SRU 1 Tailgas Valve to the TGCU and then
through the TGCU Warmup/Bypass Valve.
(2) Through the SRU 1 Tailgas Valve to the TGCU and then
through the TGCU Reactor Feed Heater, the TGCU Reactor,
the TGCU Waste Heat Reclaimer, and the TGCU Start-Up
Blower.
C. If the second SRU (Train 2) is also ready to send its tailgas to the
TGCU, toggle the SRU 2 "fast" transfer switch in the DCS to repeat
these actions for the other SRU.
For this scenario, the opening and closing of Tailgas Valves to the
TGCU and the Tailgas Valves to the TTO in Steps B and C can
occur rapidly with no impact on either the SRU or the TGCU. This is
because the TGCU Warmup/Bypass Valve will still be open at this
Note: The “fast” transfer switches can also be used to take the
Train 1 SRU and/or Train 2 SRU tailgas out of the TGCU.
Every other toggle of these selector switches will take the
opposite action to open the tailgas valve to the TTO and
then close the tailgas valve to the TGCU.
D. Slowly reduce the output from the hand control to 0% to close the
TGCU Warmup/Bypass Valve.
Now all of the SRU tailgas must flow through the TGCU Reactor
Feed Heater, etc. as this is the only open flowpath to the TTO.
E. With the SRU tailgas flowing through the TGCU Reactor Feed
Heater, the re-circulation from the TGCU Start-Up Blower is no
longer needed.
Shut down the TGCU Start-Up Blower using the start/stop selector
switch in the DCS.
(1) The TGCU Start-Up Blower bypass valve is opened and proved
open.
(4) The TGCU Start-Up Blower Suction Valve and the TGCU
Start-Up Blower Discharge Valve are closed.
Confirm that these valves have moved to the proper positions and
that the blower has stopped.
F. Place the nitrogen flow controller in "manual" and set its output to 0%
to close the control valve and stop the flow of nitrogen into the
TGCU.
At this point, all of the tailgas from both SRUs is flowing into the
TGCU Reactor Feed Heater, mixing with the external reducing gas in
the TGCU Reactor Feed Mixer, entering the TGCU Reactor to
convert all of the sulfur compounds to H2S, being cooled in the
TGCU Waste Heat Reclaimer, and flowing through the TGCU
Quench Column Bypass Valve and the TGCU Start-Up Blower
Bypass Valve to the Thermal Oxidizer via the TGCU Contactor
overhead line and the TGCU Outlet Valve.
Then, once the SRU 1 Tailgas Valve to the TGCU was fully open, the
SRU 1 Tailgas Valve to the TTO would begin to close. This would
begin forcing all of the Train 1 tailgas and Train 2 tailgas into the
TGCU Reactor Feed Heater. The outlet temperature from it would
begin to drop while the controls began increasing the steam flow rate
to the heater. Once the SRU 1 Tailgas Valve to the TTO was fully
closed, all of the Train 1 and Train 2 tailgas would be flowing to the
TGCU Reactor Feed Heater, causing an abrupt increase in its
operating pressure from about 0.07 kg/cm2(g) to about 0.3 kg/cm2(g).
This would cause the air and acid gas flow rates to the SRUs to
suddenly drop, possibly causing the SRUs to flame-out. If so, the
SRUs and the TGCU would shut down and the operators would have
to start over again.
If the SRUs and TGCU did manage to stay on-line, the TGCU
Reactor Feed Heater would only be supplying about half as much
heating as needed until the controls recover and bring the steam flow
rate up to the new requirements. Until the controls recover, the inlet
temperature to the TGCU Reactor would be low, possibly causing
incomplete conversion of SO2 in the reactor and allowing SO2 to
reach the quench water system and foul it. The reducing gas flow
rate might also require time to adjust to the higher tailgas flow rate,
further compounding the problems with conversion in the reactor.
So, the best that could be expected if the second SRU is routed to
the TGCU in the same manner as under the first scenario is an upset
in both SRUs, the TGCU Reactor Feed Heater, the TGCU Reactor,
and the quench water system. Depending on how quickly the SRUs
respond to sudden changes in operating pressure, the SRU burners
might flame-out. In this worst case, a complete restart of the SRUs
and the TGCU would then be required.
Instead of introducing the tailgas from the second SRU into the
TGCU in an abrupt manner, what is needed is a slow, controlled
redirection of the tailgas from the TTO to the TGCU. This can be
accomplished by the DCS operator using the hand controls for the
SRU 1 Tailgas Valve to the TTO and the SRU 1 Tailgas Valve to the
TGCU.
Under this scenario, the TGCU is already processing tailgas from the
Train 2 SRU. This means that the TGCU warmup/bypass valve is
already closed. This signals the PLC to disable the "fast" transfer
switches in the DCS, so that the rapid switching sequence
(scenario 1) cannot be activated inadvertently.
A. Initiate the over-ride for the Train 1 tailgas valves by toggling the
Train 1 "slow" transfer switch in the DCS, to "OVER-RIDE". The PLC
temporarily removes the limit switches on the SRU 1 Tailgas Valve to
the TTO and the SRU 1 Tailgas Valve to the TGCU from the
"complete flowpath interlock" for the Train 1 SRU alarms and
deactivates the "valve malfunction" alarms on these two valves, then
directs the DCS to release control of the hand controls for these
valves to the operator.
B. Use the hand control to slowly begin throttling the tailgas flow with
the SRU 1 Tailgas Valve to the TTO, so that the pressure at the
front-end of Train 1 is slightly higher than at the front-end of the
Train 2 SRU. Monitor the flows and pressure in the Train 1 SRU and
adjust the hand control accordingly.
C. Once the SRU 1 Tailgas Valve to the TTO is throttling, use the other
hand control to slowly open the SRU 1 Tailgas Valve to the TGCU.
Some of the Train 1 tailgas may begin to flow into the TGCU at this
time, but most of it will still flow through the SRU 1 Tailgas Valve
directly to the TTO. Monitor the flows and pressures in the Train 1
SRU and the TGCU, and adjust the rate at which he opens the SRU
1 Tailgas Valve to the TGCU accordingly.
D. Once the SRU 1 Tailgas Valve to the TGCU is fully open, use the
hand control to slowly close the SRU 1 Tailgas Valve to the TTO the
rest of the way and send all of the Train 1 tailgas to the TGCU.
Monitor the flow rates and temperatures in the TGCU, and adjust the
rate at which he closes the SRU 1 Tailgas Valve to the TTO as
needed to allow time for the controls in the TGCU to respond.
E. Once the SRU 1 Tailgas Valve to the TTO is fully closed, the Train 1
SRU is flowing to the TGCU along with the Train 2 SRU, and the
TGCU is fully on-line.
Once both valves have moved into position, the PLC will
automatically restore the limit switches on the SRU 1 Tailgas Valve
to the TTO and the SRU 1 Tailgas Valve to the TGCU to the
"complete flowpath interlock" in the SRU alarms, restore the
malfunction alarms for these valves to their normal configurations,
and reset the "slow" transfer switch in the DCS, back to "NORMAL"
and remove the over-ride.
One further point to note is that the "slow" transfer over-ride switches
can also be used to "back" tailgas out of the TGCU. If the operator
wants to shut down the TGCU in a controlled fashion, this can be
accomplished by using the TGCU Startup Blower to circulate gas
through the TGCU Reactor Feed Heater while slowly "backing" the
SRU tailgas out of the TGCU. The steps to perform this are
essentially the same as those listed above (but in reverse order).
A. The quench water system should be charged with its initial fill of
water, so that the level in the TGCU Quench Column is at the normal
setpoint for the Quench Column level controller.
E. The TGCU Quench Water Filter should be in service with the filtered
quench water flow controller controlling at its normal setpoint.
G. The amine system should be charged with its initial fill of amine, with
the level control in the DCS controlling the level in the TGCU
Contactor at its normal setpoint.
J. The fans should be operating on the TGCU Lean Amine Cooler, with
the temperature controller on the lean amine controlling at its normal
setpoint or lower.
Before introducing process gas into the TGCU columns, confirm that the
following conditions are all true:
If any of these conditions are not true, do not proceed until correcting the
problem(s). Once all of these conditions are satisfied, complete the
startup of the TGCU as follows:
A. Confirm that the Quench Column hand control in the DCS is set to
0% output with the TGCU Quench Column Inlet Valve closed and the
TGCU Quench Column Bypass Valve open.
B. Use the drain valve downstream of the TGCU Waste Heat Reclaimer
to drain any liquids that may have accumulated in the TGCU Quench
Column inlet line.
C. Slowly increase the output from the Quench Column hand control to
100%, which will open the Quench Column inlet valve and admit
process gas to the TGCU Quench Column, then close the TGCU
Quench Column Bypass Valve to prevent gas from bypassing to the
Thermal Oxidizer.
Note that the pressure drop through the TGCU Quench Column and
the TGCU Contactor will raise the operating pressures of the SRU
and the TGCU and can affect the process gas flow rates, so allow
time for the flow and flow-ratio control loops to respond.
D. When the output of the Quench Column hand control reaches 100%,
the Quench Column inlet valve should be fully open and the TGCU
Quench Column Bypass Valve fully closed to send all of the process
gas into the TGCU Quench Column. Visually confirm that these
valves are properly positioned.
E. As process gas flows into the columns, watch the operation of the
quench water system carefully. It is typical to see a slow decrease in
the quench water pH as H2S in the process gas dissolves into the
water, but a rapid decline in pH could indicate SO2 in the process
gas from incomplete reaction in the TGCU Reactor. Be ready to add
caustic if needed to keep the pH above 7.
NOTE: The quench water will probably turn black or green on this
first introduction of H2S into the system (due to small
particles of iron sulfide in the water). The TGCU Quench
Water Filter should clear up the water in a few hours.
G. Once the columns are operating stably, switch the H2/H2S analyzer
to take its sample from the TGCU Contactor overhead line by
checking that the sample line is clear of liquid, confirming that the
sample valve on the overhead line is open, and switching the sample
selector valve in the analyzer enclosure to sample from the TGCU
Contactor overhead line. (Note that the sample line on the outlet
from the TGCU Waste Heat Reclaimer is now being back-purged
with nitrogen.)
The gas stream from the TGCU Contactor is "cleaner" than the one
leaving the TGCU Waste Heat Reclaimer and is less likely to cause
problems in the hydrogen analyzer. However, if the Quench Column
hand control is used to divert gas to the TTO during an upset as
H. Once the operation of the TGCU Stripper has stabilized, route its
acid gas, which is presently going to the flare through a pressure
valve, back to the SRUs as follows:
(1) Confirm that the TGCU Stripper pressure controller to the SRUs
in the DCS is in "manual" with its output set to 0%.
(4) If, necessary, adjust the setpoint of the TGCU Stripper pressure
controller to the SRU to its normal setpoint.
The TGCU Stripper pressure controller will now take over control of
the TGCU Stripper pressure by opening the pressure valve to send
the acid gas to the Acid Gas Knock-Out Drums in the SRUs. The
TGCU Stripper pressure controller to the flare will close the acid gas
pressure valve and stop the flow of acid gas to the flare. If the SRUs
shut down (or some other upset causes the TGCU Stripper pressure
to rise), the TGCU Stripper pressure controller to the flare will act as
an over-ride and divert the acid gas to the flare.
(2) Lower the setpoint of the temperature control on the lean amine
to maximize the aerial cooling. This will cool the amine to the
TGCU Contactor as much as possible to maximize the amine
selectivity and treating ability.
The aerial coolers and trim coolers will not be able to maintain these
temperatures when the ambient conditions are very warm, of course.
However, setting the controllers this way will keep the fan speed high
to maximize cooling at all times.
(1) Both SRU Tailgas Valves to the TTO and the TGCU
Warmup/Bypass Valve are fully closed (to prevent leakage of
SRU tailgas to the Thermal Oxidizer that would cause high SO2
emissions and the resulting permit violation).
(2) The TGCU Quench Column Bypass Valve is fully closed (to
prevent leakage of TGCU Reactor effluent to the Thermal
Oxidizer that would cause high SO2 emissions and the resulting
permit violation).
(4) The steam heating systems are in service on the jacketed sulfur
vapor valves and the steam traps are functioning properly.
(2) If any of the flanged connections in the TGCU were opened for
maintenance or other purposes while the TGCU was off-line, it
is good practice to leak test the TGCU before returning it to
service. Refer to Section 11.7.5 of these guidelines for a
suggested procedure to accomplish this.
(3) Place all the steam heating systems on the sulfur vapor valve
jackets in service. Check all steam traps for proper operation,
and use the vent valves to sweep non-condensibles out of the
steam spaces.
E. Verify that the automated shutdown valves, the block valves, and
the downstream steam-jacketed block valve in the reducing gas
line to the TGCU Reactor Feed Mixer are all closed.
J. Confirm that the Quench Column hand control in the DCS is set
to 0% output, so that the TGCU Quench Column inlet valve will
remain fully closed and the TGCU Quench Column bypass
valve will open later in when the TGCU startup/run selector
switch is switched to "STARTUP".
L. Visually confirm that both SRU Tailgas Valves to the TGCU are
closed.
P. Verify that the local stop control for the TGCU Start-Up Blower
is set to the "RUN" position.
Q. Check that the sample line from the outlet of the TGCU Waste
Heat Reclaimer to the hydrogen analyzer is clear of liquids.
Confirm that sample valve on the outlet channel of the boiler is
open, then switch the sample selector valve in the analyzer
enclosure to sample from the outlet of the TGCU Waste Heat
Reclaimer.
C. Set the output of the hand control in the DCS to 0% to close the
TGCU Warmup/Bypass Valve and visually confirm that the
valve is closed.
(4) After the limit switches prove these valves open, the
TGCU Start-Up Blower is started.
F. Confirm that the BFW level controller and control valve to the
TGCU Waste Heat Reclaimer are in service and functioning
properly.
(1) Confirm that the remote setpoint that the reactor feed
temperature controller is supplying to the pressure
controller matches the current setting on the pressure
controller.
If any of these conditions are not true, do not attempt to bring SRU
tailgas into the TGCU. In particular, do not attempt switching
tailgas into the TGCU when the SRU(s) is(are) experiencing an
upset. The result will be multiple upset units to deal with. Instead,
focus your attention on stabilizing the operation of the SRU(s) first
(usually by correcting a problem in the upstream Amine
Regeneration and/or Sour Water Stripper units), and then use the
procedure that follows to establish tailgas flow into the TGCU.
The first scenario to consider for introducing tailgas into the TGCU is
a normal startup of the SRUs and the TGCU. Before being routed to
the TGCU, the tailgas from both SRUs is sent to the TTO while the
TGCU uses the TGCU Startup Blower to re-circulate gas to the
TGCU Reactor Feed Heater via the TGCU Warmup/Bypass Valve.
Once the TGCU is warmed up and ready to accept tailgas, the
Train 1 and Train 2 SRUs can be routed to the TGCU as follows
(using the Train 1 SRU for this procedure).
(2) After the limit switches prove this valve open, the SRU 1
Tailgas Valve to the TTO is closed.
C. If the second SRU (Train 2) is also ready to send its tailgas to the
TGCU, toggle the SRU 2 "fast" transfer switch in the DCS to repeat
these actions for the other SRU.
For this scenario, the opening and closing of Tailgas Valves to the
TGCU and the Tailgas Valves to the TTO in Steps B and C can
occur rapidly with no impact on either the SRU or the TGCU. This is
because the TGCU Warmup/Bypass Valve will still be open at this
time, so there will be very little differential pressure across the
Tailgas Valves to the TGCU and there will not be an abrupt change
in pressure when the Tailgas Valves to the TGCU are opened or
when the Tailgas Valves to the TTO are closed.
Note: The “fast” transfer switches can also be used to take the
Train 1 SRU and/or Train 2 SRU tailgas out of the TGCU.
Every other toggle of these selector switches will take the
D. Slowly reduce the output from the hand control to 0% to close the
TGCU Warmup/Bypass Valve.
Now all of the SRU tailgas must flow through the TGCU Reactor
Feed Heater, etc. as this is the only open flowpath to the TTO.
E. Shut down the TGCU Start-Up Blower using the start/stop selector
switch in the DCS.
(1) The TGCU Start-Up Blower bypass valve is opened and proved
open.
(4) The TGCU Start-Up Blower Suction Valve and the TGCU
Start-Up Blower Discharge Valve are closed.
Confirm that these valves have moved to the proper positions and
that the blower has stopped.
F. Place the nitrogen flow controller in "manual" and set its output to 0%
to close the control valve and stop the flow of nitrogen into the
TGCU.
At this point, all of the tailgas from both SRUs is flowing into the
TGCU Reactor Feed Heater, mixing with the external reducing gas in
the TGCU Reactor Feed Mixer, entering the TGCU Reactor to
convert all of the sulfur compounds to H2S, being cooled in the
TGCU Waste Heat Reclaimer, and flowing through the TGCU
Quench Column Bypass Valve and the TGCU Start-Up Blower
Bypass Valve to the Thermal Oxidizer via the TGCU Contactor
overhead line and the TGCU Outlet Valve.
A. Initiate the over-ride for the Train 1 tailgas valves by toggling the
Train 1 "slow" transfer switch in the DCS, to "OVER-RIDE". The PLC
temporarily removes the limit switches on the SRU 1 Tailgas Valve to
the TTO and the SRU 1 Tailgas Valve to the TGCU from the
"complete flowpath interlock" for the Train 1 SRU alarms and
deactivates the "valve malfunction" alarms on these two valves, then
directs the DCS to release control of the hand controls for these
valves to the operator.
B. Use the hand control to slowly begin throttling the tailgas flow with
the SRU 1 Tailgas Valve to the TTO, so that the pressure at the
front-end of Train 1 is slightly higher than at the front-end of the
Train 2 SRU. Monitor the flows and pressure in the Train 1 SRU and
adjust the hand control accordingly.
C. Once the SRU 1 Tailgas Valve to the TTO is throttling, use the other
hand control to slowly open the SRU 1 Tailgas Valve to the TGCU.
Some of the Train 1 tailgas may begin to flow into the TGCU at this
time, but most of it will still flow through the SRU 1 Tailgas Valve
directly to the TTO. Monitor the flows and pressures in the Train 1
SRU and the TGCU, and adjust the rate at which he opens the SRU
1 Tailgas Valve to the TGCU accordingly.
D. Once the SRU 1 Tailgas Valve to the TGCU is fully open, use the
hand control to slowly close the SRU 1 Tailgas Valve to the TTO the
rest of the way and send all of the Train 1 tailgas to the TGCU.
Monitor the flow rates and temperatures in the TGCU, and adjust the
rate at which the SRU 1 Tailgas Valve to the TTO is closed to allow
time for the controls in the TGCU to respond.
E. Once the SRU 1 Tailgas Valve to the TTO is fully closed, the Train 1
SRU is flowing to the TGCU along with the Train 2 SRU, and the
TGCU is fully on-line.
Once both valve have moved into position, the PLC will automatically
restore the limit switches on the SRU 1 Tailgas Valve to the TTO and
the SRU 1 Tailgas Valve to the TGCU to the "complete flowpath
interlock" in the SRU alarms, restore the malfunction alarms for
these valves to their normal configurations, and reset the "slow"
transfer switch in the DCS, back to "NORMAL" and remove the
over-ride.
G. The amine system should be filled with amine, with the level
control in the DCS controlling the level in the TGCU Contactor
at its normal setpoint.
L. The TGCU lean amine filters should be in service, with the flow
controller controlling at its normal setpoint.
If any of these conditions are not true, do not proceed until correcting
the problem(s). Once all of these conditions are satisfied, complete
the startup of the TGCU as follows:
A. Confirm that the Quench Column hand control in the DCS is set
to 0% output with the TGCU Quench Column Inlet Valve closed
and the TGCU Quench Column Bypass Valve open.
Note that the pressure drop through the TGCU Quench Column
and the TGCU Contactor will raise the operating pressures of
the SRU and the TGCU and can affect the process gas flow
rates, so allow time for the flow and flow-ratio control loops to
respond.
(1) The SRU Tailgas Valve to the TTO and the TGCU
Warmup/Bypass Valve are fully closed (to prevent leakage of
SRU tailgas to the Thermal Oxidizer that would cause high SO2
emissions and the resulting permit violation).
(2) The TGCU Quench Column Bypass Valve is fully closed (to
prevent leakage of TGCU Reactor effluent to the Thermal
Oxidizer that would cause high SO2 emissions and the resulting
permit violation).
(4) The steam heating systems are in service on the jacketed sulfur
vapor valves and the steam traps are functioning properly.
The TGCU is affected directly and indirectly by shutdowns and outages that
occur in other systems within the Sulfur Block. The more important aspects of
the effects these other systems can have on the TGCU are discussed in
Section 11.9.6.
Typical shutdown procedures are outlined and discussed in the sections that
follow for the more common cases. Your existing company procedures and
common sense operational judgment should be used to modify these
A. Check that the sample line from the outlet of the TGCU Waste Heat
Reclaimer to the H2/H2S analyzer is clear of liquids. Confirm that
sample valve on the outlet channel of the boiler is open, then switch
the sample selector valve in the analyzer enclosure to the "START-UP"
position (taking sample from the outlet of the TGCU Waste Heat
Reclaimer).
B. Visually confirm that the TGCU Start-Up Blower Bypass Valve is fully
open and that the DCS indicates that the valve is open.
C. Slowly reduce the output from the Quench Column hand control in
the DCS to divert the process gas from the TGCU columns and send
it to the Thermal Oxidizer. The Quench Column hand control will
open the TGCU Quench Column Bypass Valve, then close the
TGCU Quench Column Inlet Valve.
D. When the output of the Quench Column hand control reaches 0%,
the TGCU Quench Column Bypass Valve should be fully open and
the Quench Column inlet valve fully closed to send all of the process
gas to the Thermal Oxidizer via the TGCU Start-Up Blower Bypass
Valve.
Some of the SRU tailgas will continue to flow through the TGCU
Reactor Feed Heater, etc. to the TTO through the TGCU Start-Up
Blower Bypass Valve, but most of the tailgas will flow instead through
the TGCU Warmup/Bypass Valve to the TTO.
I. Toggle the fast transfer switch for SRU 1 in the DCS to "CLOSE".
The PLC will open the SRU 1 Tailgas Valve to the TTO then close
the SRU 1 Tailgas Valve to the TGCU. All of the SRU 1 tailgas is
now flowing directly to the TTO via the SRU 1 Tailgas Valve, and
none of the tailgas is entering the TGCU.
J. Toggle the fast transfer switch for SRU 2 in the DCS to "CLOSE".
The PLC will open the SRU 2 Tailgas Valve to the TTO then close
the SRU 2 Tailgas Valve to the TGCU. All of the SRU 2 tailgas is
now flowing directly to the TTO via the SRU 2 Tailgas Valve, and
none of the tailgas is entering the TGCU.
The PLC will close the reducing gas block valves, open the vent
valve, and force the control valve to "manual" and 0% output.
Confirm that the DCS indicates that these valves have moved to the
proper position.
L. Close the steam-jacketed block valve in the reducing gas supply line.
M. Reduce the output from the hand control in the DCS to 0% to close
the TGCU Warmup/Bypass Valve. Visually confirm that the valve is
closed.
N. Now that the reducing gas has been isolated and the tailgas from the
SRU has been switched to the Thermal Oxidizer, allow the front-end
of the TGCU to operate in this fashion for about 15 minutes to purge
the process gas out to the Thermal Oxidizer.
O. Place the HP steam pressure controller for the TGCU Reactor Feed
Heater in "manual" and set its output to 0% to close control valve.
WARNING
(5) The reducing gas to the TGCU Reactor Feed Mixer is blocked-in
and bled.
(7) The suction and discharge valves for the TGCU Startup Blower
are closed and the nitrogen purge is in service.
(8) The TGCU Quench Column inlet valve and the TGCU Quench
Column Bypass valve are closed.
(9) All steam heating services on the sulfur vapor valve jackets are
still functioning and the steam traps are operating properly.
V. Continue to circulate the TGCU amine and operate the TGCU Lean
Amine Cooler, the TGCU Lean Amine Trim Cooler, and the TGCU
Stripper Reflux Condenser until the amine is cool.
W. Once the amine is cool (60°C or less throughout the system), shut
down the equipment in the following order:
(5) The fans on the TGCU Quench Water Cooler, TGCU Lean
Amine Cooler, and TGCU Stripper Reflux Condenser.
Close the steam outlet valve on the boiler and open the vent valves
on the boiler to de-pressure it. Make sure that the boiler level control
continues to operate properly so that the water level does not drop
below the tubes until they have cooled and the boiler is fully
de-pressured. Once the boiler is de-pressured, block-in its BFW
supply and drain the water from it. Then use a temporary "jumper" to
supply LP steam to the boiler shell. Drain the condensate from the
boiler occasionally to keep the tubes safely above the water
condensation temperature (100-110°C).
There are service companies, however, that can unload the TGCU
catalyst bed after it has been cooled to near ambient temperature using
nitrogen. The service company then performs all necessary work relating
to removing and replacing the catalyst under a nitrogen "blanket". This
eliminates the need to passivate the catalyst, reducing the time required to
replace the TGCU catalyst. Some refineries and gas plants also purchase
pre-sulfided replacement catalyst, resulting in less time for the subsequent
startup.
The procedure in this section is used to make the TGCU catalyst safe for
atmospheric air replacement.
NOTE: Do not drain the water from the TGCU Waste Heat
Reclaimer (Step X in Section 11.9.1). The boiler and its
BFW controls must remain in service until the completion
of the catalyst passivation procedure.
B. Confirm that the TGCU Outlet Valve is open and start a small
nitrogen purge into the bottom of the TGCU Quench Column. (This is
typically done by hooking up a temporary jumper to a connection on
one of the level bridles.)
This will purge through both the TGCU Quench Column and the
TGCU Contactor and ensure that the SO2 formed during passivation
does not contaminate the quench water or the amine.
D. Visually confirm that the TGCU Start-Up Blower suction block valve
and discharge block valve are closed, the bypass valve is open, the
nitrogen purge to the blower seal is in service, and the local "stop"
control at the blower is set to the run position.
E. Start the TGCU Start-Up Blower using the start/stop toggle switch in
the DCS.
(4) After the limit switches prove these valves open, the TGCU
Start-Up Blower is started.
(5) Once the Startup Blower is started, the TGCU Start-Up Blower
Bypass Valve is closed.
As this valve is closed, the blower will start to load. As it does so, the
blower will begin to "pull" nitrogen through the TGCU Reactor Feed
Heater and TGCU Reactor Feed Mixer and all of the associated
piping.
H. Allow the front-end of the TGCU to operate in this manner until the
following conditions are both satisfied:
I. Verify that the utility air flow controller is in "manual" and set to 0%
output.
J. Verify that flow control valve, the upstream block valve, and the
downstream block valve are all closed in the utility air supply line.
K. Rotate the spectacle blind in the utility air line to the "open" position,
then open the upstream block valve and the downstream block valve.
L. Slowly increase the output from the flow controller to open the flow
valve and admit a small amount of utility air into the circulating gas
and begin passivating the catalyst. A maximum oxygen
CAUTION
N. When there is no longer any temperature rise across the reactor, the
passivation of the catalyst is complete. Discontinue the flow of
nitrogen to the front-end of the TGCU by placing the nitrogen flow
controller in "manual" and setting its output to 0% to close the control
valve. Observe the TGCU Reactor temperatures to ensure that no
further reaction occurs (leave the nitrogen flowing to the TGCU
Quench Column).
If the catalyst bed temperatures start to rise when the nitrogen flow is
discontinued, re-establish nitrogen flow until the bed cools again,
then stop the nitrogen flow. Repeat this step as necessary until there
is no temperature rise in the reactor with the nitrogen flow shut off.
O. Once the nitrogen flow has been discontinued, the TGCU Start-Up
Blower is no longer needed for re-circulation. Shut down the blower
as follows:
(1) Reduce the output from the hand control to 0% to close the
TGCU Warmup/Bypass Valve and stop the recycle flow to the
TGCU Reactor Feed Heater.
Verify that the valve has closed, and that the DCS indicates that
this valve has closed.
(2) Shut down the blower using the start/stop selector switch in the
DCS.
The PLC will open the TGCU Blower Bypass Valve, stop the
blower, turn on the nitrogen purge, and close its suction and
discharge valves. Verify that the DCS indicates each valve has
moved to the proper position.
P. Use the flow controller to raise the utility air flow to 80% or more and
allow air to cool the TGCU Reactor.
Continue the air flow until the temperature leaving the TGCU Reactor
is about the same temperature as the air entering the TGCU
Reactor.
R. Close the upstream block valve and the downstream block valve in
the utility air supply line, then rotate the spectacle blind to the
"closed" position. Close the steam-jacketed block valve at the
junction with the tailgas line to the TGCU Reactor Feed Heater.
WARNING
(4) The nitrogen to the TGCU Reactor and the TGCU Quench
Column is positively isolated from the TGCU.
(6) The TGCU Start-Up Blower is shut down, with its suction and
discharge valves closed and the nitrogen purge in service.
(7) The TGCU Quench Column inlet valve and the TGCU Quench
Column bypass valve are closed.
(8) All steam heating services on the sulfur vapor valve jackets are
still functioning and the steam traps are operating properly.
U. The TGCU catalyst is now passivated and cooled, and can be safely
handled. The TGCU is now ready to be isolated and made safe for
entry.
Close the steam outlet valve on the boiler and open the vent valves
on the boiler to de-pressure it. Make sure that the boiler level control
continues to operate properly so that the water level does not drop
below the tubes until they have cooled and the boiler is fully
de-pressured. Once the boiler is de-pressured, block-in its BFW
supply and drain the water from it. Then use a temporary "jumper" to
supply LP steam to the boiler shell. Drain the condensate from the
boiler occasionally to keep the tubes safely above the water
condensation temperature (100-110°C).
A. Switch the SRU tailgas from the TGCU to the Thermal Oxidizer.
E. Maintain a visible water level in the boiler. Water must remain in the
boiler until it is de-pressured to prevent overheating damage to the
tubes.
F. Once the boiler is fully de-pressured, drain the water from the boiler
to prevent any further leakage into the process side of the
equipment.
G. The TGCU is now ready to be isolated and made safe for entry.
CAUTION
When a TGCU is shut down for any appreciable length of time, water
vapor in the process gas can condense and accumulate in the low spots.
Since the process gas contains CO2, H2S, SO2, and other compounds, the
condensed water can be quite acidic. As this acid water trickles over the
piping, it corrodes the metal. If this water then reaches a steam-jacketed
valve or pipe, the water will boil away and deposit the corrosion products
on the heated surface. This occurrence can quickly cause a
steam-jacketed valve to become "stuck", which usually results in an
extended shutdown to repair the valve before that TGCU can be restarted.
The most positive means for preventing condensation of water in the unit
is to purge it with inert gas (nitrogen, etc.). One way to accomplish this is
as follows:
A. Confirm that the Quench Column hand control in the DCS is set to
0% output.
C. Confirm that the Leak Test switch in the DCS is toggled to "OFF".
The PLC will open the TGCU Quench Column Bypass Valve. Verify
that the DCS indicates that the Quench Column Bypass Valve is
open.
G. Verify that the TGCU Start-Up Blower Bypass Valve is open and that
the DCS indicates that the valve is fully open.
J. Place the nitrogen flow controller in "manual" and adjust its output to
open the control valve slightly and establish a small flow of nitrogen
into the front-end of the TGCU.
K. "Crack" the TGCU Outlet Valve open slightly to allow the nitrogen to
flow to the Thermal Oxidizer. Adjust the TGCU Outlet Valve to
"pinch" so that the pressure in the TGCU is slightly positive (about
0.07-0.15 kg/cm2(g)) on the pressure indicator in the DCS.
L. With the valves arranged in this manner, the purge gas will proceed
as follows:
(1) Through the TGCU Rector Feed Heater, TGCU Reactor Feed
Mixer, TGCU Reactor, and TGCU Waste Heat Reclaimer.
(4) Through the TGCU Contactor overhead line, flowing past the
TGCU Warmup/Bypass Valve.
(5) Through the TGCU Outlet Valve and out to the Thermal
Oxidizer.
This will keep purge gas sweeping through or past all of the
steam-jacketed process gas valves so that condensed water will not
accumulate and cause problems.
If it is not possible to purge the TGCU with inert gas while it is shut
down, it is possible to protect these valves by using drain valves to
prevent the accumulation of water near the steam-jacketed valves.
In order to accomplish this, drain valves in the following locations are
used:
WARNING
A. Confirm that the SRU Tailgas Valves to the TGCU are closed.
B. Close the TGCU Outlet Valve. Make sure that this valve is
closed tightly.
However, if the TGCU is not yet processing tailgas from either SRU,
there is no reason to shut it down if the SRUs are not running. This
simplifies startup of the TGCU by allowing its ESD system to be
independent of the SRU ESD systems until tailgas is introduced into
the TGCU.
If the H2S concentration in the TTO feed gas is high (above 3.0%),
do not attempt to restart the Thermal Oxidizer. Instead, direct your
attention to the amine or SWS unit upstream of the SRUs that is
probably causing the problem and bring the SRUs back on-ratio.
This will allow the TGCU to reduce the H2S concentration in the
Thermal Oxidizer feed gas to an acceptable level, so that restart of
the Thermal Oxidizer can proceed smoothly.
4. The H2S content of the TGCU Contactor overhead gas (Sections 11.10.6
and 11.10.7).
1
The Dow Chemical Company, Gas Conditioning Fact Book, 1962, pp. 310-311.
2
Dow Chemical U.S.A., Gas Treating from Dow, 1987, pp. 8-1-1 – 8-1-2.
Heat stable salts can also be determined by a total anion assay. The
amine solution is passed through an ion exchange column containing ion
exchange resin in the hydrogen form. Acid salts are thus broken down
and the acids recovered in the column effluent, while the amine is
absorbed in the column. The acid in the effluent is determined by
potentiometric titration, and from these results plus the original amine
concentration the amount of amine in the form of heat stable salts is
calculated. Again, this type of analysis is commonly left for the chemical
solvent supplier to perform.
Steps should be taken to ensure that the amine solution samples taken
are representative of the circulating solvent. Samples should be taken in
glass or plastic containers. Metal containers will cause low results for H2S
because sulfides will react with the metal walls of the container. Do not
use copper tubing to withdraw the samples; the copper will contaminate
the amine solution, and H2S will react with the copper and give low
results.
Special care should be exercised when taking samples of the rich amine
solution to avoid personnel exposure to H2S. Hot, fully loaded amine
solution can flash acid gas when released to atmospheric pressure,
causing low acid gas loading results in addition to the dispersion of H2S to
the surroundings. Take samples of the rich solution from the coolest point
in the process (the TGCU Contactor outlet, usually), and cool the samples
in a stainless steel coil immersed in an ice bath or cold water to prevent
flashing. The solution should be allowed to flow to a drain in this fashion
for several minutes before taking the sample to be sure that circulating
amine is being taken.
2. Procedure:
d. Titrate the solution in the beaker with 0.5 N HCl to a faint yellow
color. Alternatively, if a pH meter is available, titrate to a pH of
4.5. Record the amount of HCl used in the titration.
2. Procedure:
hydrogen carbonate salts. Once all of the acid gas has reacted, the
continued addition of base causes the pH of the solution to rise, until
the Thymolphthalein indicator changes from colorless to blue. Note
that KOH reacts with H2S and CO2 on a 1:1 molar basis.
Note that "ml KOH used" refers to the amount used in the second
titration, step 2.e. The "wt % amine in solvent" can be determined
using the procedure in Section 11.10.2.
5. Special Considerations:
2. Procedure:
H2S + I2 S + 2 HI
When the solvent is added to the iodine solution, the H2S in the
solvent reacts with the iodine to form hydrogen iodide and elemental
sulfur. The solution contains an excess of iodine to ensure that all of
the H2S reacts. The iodine solution is chilled prior to adding the
solvent to eliminate or minimize the evolution of H2S gas. Note that
H2S reacts with iodine on a 1:1 molar basis.
g - moles g - moles
Amine I2 Used Na2S2O3 Used
Mole 100 %
Moles H2S
Mole Amine Weight ml of S.G. of Wt % Amine
Sample Sample in Solvent
Normality Normality of
ml I2 of I ml Na2S2O3 Na S O
Used 2 Used 2 2 3
Moles H2S Solution Solution
5.626
Mole Amine ml of Wt % Amine
Sample in Solvent
Using the total acid gas loading determined with the procedure in
Section 11.10.3, the CO2 loading of the solvent is determined by
difference:
Moles H2S
Wt % Amine
Wt % H2S 0.2858
Mole Amine in Sample
Moles CO2
Wt % Amine
Wt % CO2 0.3693
Mole Amine in Sample
1. Principle:
3. Procedure:
c. Start the air pump or air supply to agitate the sample with
oil-free air at 4 liters per minute (0.2 Nm3/H).
d. After five minutes, record the height of the foam in the cylinder
(in ml). Then turn off the air supply and measure the time in
seconds for the foam to "break". For consistency, foam "break"
is defined as the first clear "fish eye" in the surface of the liquid
in the cylinder.
4. Calculation:
5. Interpretation:
Considerable experience with this test has shown that if the foam
height exceeds 200 ml or the "break" time exceeds 5 seconds, the
plant may be experiencing a foaming problem. The higher the foam
height and/or the longer it takes to "break", the more severe the
problem.
6. Other Considerations:
H2S + I2 2 HI + S
The Normality of the standard iodine solution will be 0.1 N. The last
three factors (which correct the actual H2S content to compensate for
expansion due to temperature, pressure, and water content) can be
combined and calculated as a function of temperature only. This has
been done for the 500-ml gas sample and is included as the
Tutweiler Factor Chart in Section 9.10 of these guidelines (Chart 2).
Therefore, the equation above can be simplified to:
11.10.7 H2S Conc. in TGCU Contactor Ovhd Using Gas Detector Tubes
As an alternative to the traditional wet-chemistry method described in the
preceding Section 11.10.6 for determining the concentration of H2S in the
TGCU Contactor overhead gas, gas detector tubes can be used to quickly
and easily make this determination. Although the discussion that follows
specifically addresses using gas detector tubes manufactured by
Drägerwerk AG of West Germany, there may be suitable detector tubes
available from other manufacturers. Dräger tubes can be purchased from
most safety equipment supply companies.
3. Break off the tips at each end of a Dräger tube and insert it into
the sample pump (with the arrow on the side of the tube pointing
toward the pump).
5. Stroke the sample pump one time (be sure to compress the
bellows until reaching the stops) and allow the pump to draw the
gas sample into the detector tube. The sample stroke is
complete when the metal chain on the bellows is taut.
6. Close the sample valve and remove the rubber tubing from the
end of the Dräger tube and from the sample valve.
7. Read the length of the brown stain using the marks on the tube
and record the reading.
11.10.7.3 Calculations
Mole (or Volume) PPM H2S (wet basis):
PPM H2S
Stain
Tube 1013
Length Factor Baro. Pres., mbar
The last factor corrects the measurement for pressure effects when
samples are taken at elevations above sea level. Note that the
average barometric pressure at the complex is
14.7 PSIA = 1013 mbar.
The "Tube Factor" depends on the type of Dräger tube used and the
number of sample strokes:
CO + H2O H2 + CO2
The first reaction is the classic "water gas shift" reaction. Since this is an
equilibrium reaction, an equilibrium constant for the reaction can be
expressed in terms of the reactant and product concentrations:
Keq
H2CO2
COH2O
This equilibrium constant is mainly a function of temperature. Since the
TGCU Reactor outlet temperature for a given plant is fairly constant, as
are the concentrations of CO2 and H2O in the process gas, then the ratio
of CO to H2 in the TGCU Reactor effluent should remain fairly constant as
long as the catalyst activity does not change.
Keq
H2SCO2
COSH2O
Since the temperature, H2S concentration, H2O concentration, and CO2
concentration of the TGCU Reactor outlet should all be fairly constant,
then the COS concentration of the gas leaving the TGCU Reactor should
be fairly constant.
The CO/H2 ratio is usually plotted as PPM CO divided by % H2, and the
COS is usually plotted as PPM. From the discussions above, it is clear
that a trend upward in either value, CO/H2 ratio or COS concentration,
indicates lower catalyst activity. Shell suggests planning to replace the
catalyst within a few months once either value begins to rise rapidly. Note
that the sample for the chromatograph can be taken from the gas leaving
the TGCU Quench Column, since the H2, CO, and COS concentrations
(on a dry basis) will be the same there as those leaving the TGCU
Reactor. Because this gas stream is cooler and contains less water, it is
often easier to sample and analyze than the TGCU Reactor effluent.
Table of Contents
12. TAILGAS THERMAL OXIDIZER ............................................................................ 12-2
12.1 PURPOSE OF SYSTEM ..................................................................................... 12-2
12.2 SAFETY ............................................................................................................... 12-2
12.3 PROCESS DESCRIPTION.................................................................................. 12-3
12.4 EQUIPMENT DESCRIPTION .............................................................................. 12-4
12.4.1 Thermal Oxidizer, A2-BA1570 ...................................................................... 12-4
12.4.2 Thermal Oxidizer Burner, A2-BA1571 .......................................................... 12-4
12.4.3 Steam Knock-out Drum, A2-FA1570 ............................................................ 12-4
12.4.4 Thermal Oxidizer Air Blower, A2-GB1570A/B .............................................. 12-4
12.4.5 Thermal Oxidizer Vent Stack, A2-ME1570 ................................................... 12-5
12.4.6 Refractory for Thermal Oxidizer, A2-MR1570 .............................................. 12-5
12.4.7 Thermal Oxidizer Waste Heat Boiler, A2-BF1570 ........................................ 12-5
12.5 INSTRUMENTATION AND CONTROL SYSTEMS ............................................. 12-7
12.5.1 Thermal Oxidizer Burner Management System ........................................... 12-7
12.5.2 Thermal Oxidizer Temperature Control ...................................................... 12-10
12.5.3 Thermal Oxidizer Excess Oxygen Control.................................................. 12-10
12.5.4 Boiler Low-Low Level S/D Transmitter Testing .......................................... 12-11
12.5.5 Thermal Oxidizer Shutdown System .......................................................... 12-13
12.6 PROCESS PRINCIPLES AND OPERATING TECHNIQUES ........................... 12-18
12.6.1 Equipment Damage .................................................................................... 12-18
12.6.2 Effect of Upstream Operations on the Thermal Oxidizer ............................ 12-21
12.6.3 "Swapping" Air Blowers During Operation .................................................. 12-23
12.6.4 Boiler Water Treatment .............................................................................. 12-24
12.7 PRECOMMISSIONING PROCEDURES ........................................................... 12-26
12.7.1 Preliminary Check-out ................................................................................ 12-26
12.7.2 Shutdown System Check-out ..................................................................... 12-27
12.7.3 Commissioning Fuel Gas, Pilot Gas, and I/A to the Process ..................... 12-28
12.8 STARTUP PROCEDURES................................................................................ 12-33
12.8.1 Initial Firing / Refractory Cure-out............................................................... 12-33
12.8.2 Normal Startup ........................................................................................... 12-48
12.9 SHUTDOWN PROCEDURES ........................................................................... 12-58
12.9.1 Planned Shutdown - No Entry .................................................................... 12-59
12.9.2 Planned Shutdown for Entry ....................................................................... 12-61
12.9.3 Shutting Down When Boiler Tubes Are Leaking ........................................ 12-65
12.9.4 Emergency Shutdown ................................................................................ 12-66
12.9.5 Effects of Shutdowns and Outages in Other Systems................................ 12-69
12.2 Safety
WARNING
When the TGCU is operating, the TGCU effluent containing H2S and COS flows
to the Thermal Oxidizer, A2-BA1570, at about 39°C [102°F]. When the TGCU
Unit is not in service, tailgas from each SRU containing H2S, SO2, COS, CS2,
and elemental sulfur flows directly to the Thermal Oxidizer at about 156°C
[313°F]. The spent degassing air from the Sulfur Degassing Unit and the sweep
air streams from each Sulfur Surge Tank (both containing traces of H2S and
sulfur vapor) are also routed to the Thermal Oxidizer. In the Thermal Oxidizer,
essentially all of the sulfur compounds are incinerated to SO2 by the
high-temperature oxidizing atmosphere created inside the Thermal Oxidizer. In
addition, most of the carbon monoxide (CO) in the feed stream is oxidized to
carbon dioxide, resulting in very low CO emissions from the Tailgas Thermal
Oxidation system.
The effluent from the Thermal Oxidizer flows to the Thermal Oxidizer Waste
Heat Boiler, A2-BF1570. The gas is cooled to about 288°C [550°F] as it
generates and superheats steam at 45.0 kg/cm2(g) [640 PSIG], which is
exported to the HP steam header at about 400°C [752°F] for use as motive
steam to the Sulfur Pit Ejector and for use elsewhere in the refinery. (Note that
the HP steam produced in each SRU is also superheated in this boiler by
combining it with the steam this boiler generates.) The cooled effluent is then
dispersed to the atmosphere from the top of the Thermal Oxidizer Vent Stack,
A2-ME1570.
The refractory lining inside the furnace includes a "choke ring" located
about two-thirds of the way down the length of the furnace. The purpose
of the choke ring is to promote mixing between the TGCU effluent gas (or
SRU tailgas) and the hot combustion products from the Thermal Oxidizer
Burner, ensuring efficient oxidation of the sulfur compounds and carbon
monoxide that are present in the tailgas.
The main boiler tube section contains tubes connecting the steam drum
on top of the boiler to the mud drum on the bottom of the boiler, as well as
side wall tubes. The screen section contains rows of tubes also
connected to the mud and steam drums. The hot gas entering the boiler
casing boils water as it circulates in the screen and main boiler tubes,
generating 48.5 kg/cm2(g) saturated steam.
The saturated steam generated in the boiler tubes exits the steam drum at
and is combined with saturated HP steam generated by the Waste Heat
Boilers in the SRUs. The combined steam is routed to the first
superheater section, then to the first desuperheater, and then to the
second superheater section. The resulting superheated steam is routed to
the second desuperheater and then to the HP steam header at about 45
kg/cm2(g) and 400°C.
(1) Before attempting ignition of the burner, any process gas from
the SRUs and/or TGCU Unit should be blocked from flowing
into the Thermal Oxidizer in case the process gas is
combustible. Setting selector switch A2-HS15785 on the local
TTO control panel to "STARTUP" will open the bypass valve,
A2-HV15741, prove the valve open, then close the inlet valve,
A2-HV15740, so that the process gas is diverted directly to the
Thermal Oxidizer Vent Stack.
(2) Once the pilot burner in the Thermal Oxidizer Burner has been
lit, process gas can then be directed into the Thermal Oxidizer.
Setting selector switch A2-HS15785 to "RUN" will automatically
open the inlet valve, prove the valve open, then close the
bypass valve.
If either of the switching valves does not move to the proper position,
the corresponding status light on the local TTO control panel should
continue to blink. This will alert the operators to investigate the
problem and take any required corrective action so that the BMS
allows proceeding.
to the pilot will remain open. Otherwise, the air and fuel gas supplies
to the pilot are blocked-in and the purge cycle must be repeated.
Note that the main fuel gas control valve has a minimum firing rate,
as set by the "minimum fire" relay in the DCS, A2-TY15749. The
proper setting for A2-TY15749 will be determined during startup by
finding the minimum firing rate to maintain a stable flame on the main
fuel gas burner.
If the burner is "off " (and the "flame proven" is already satisfied by
the main burner tip), pressing this push-button will ignite the burner
by closing the valve to cease purging the burner with air, closing the
vent valve and opening the two block valves in its fuel gas supply,
opening the block valve in its air supply, and energizing A2-BX15758
for 15 seconds.
(1) The outside operator notifies the DCS operator that he is preparing
to test shutdown level transmitter A2-LT15150A on the Thermal
Oxidizer Waste Heat Boiler.
(2) The DCS operator confirms that A2-LI15150B and A2-LI15150C are
both indicating adequate level in the boiler, then notifies the outside
operator to proceed.
CAUTION
(3) After being notified to proceed by the DCS operator, the outside
operator blocks-in A2-LT15150A by closing its block valves, then
opens the drain valve on the bottom of the transmitter to drain the
water from the instrument.
(4) If the transmitter is operating properly, the DCS will alarm that there
is a low level in the Thermal Oxidizer Waste Heat Boiler on
A2-LI15150A. The DCS operator acknowledges the alarm on the
DCS and reports it to the outside operator.
(5) After being notified of the alarm, the outside operator closes the drain
valve on A2-LT15150A, slowly opens its bottom block valve to allow
the transmitter to fill with water then opens its top block valve. This
should clear the low level alarm on A2-LI15150A in the DCS.
(6) After confirming that the low level alarm has cleared, the other level
transmitters can be tested in a similar fashion.
NOTE: The DCS operator must not begin another task until confirming
that the low level alarm has cleared. This is to guard against
having a level transmitter malfunction that causes a TTO ESD
when the other transmitters are tested.
12.5.5.1 Causes
Any one of the causes listed below will activate the TTO ESD
system:
Loss of air flow from the Thermal Oxidizer Air Blower could
cause the Thermal Oxidizer Burner flame to become unstable,
or allow TGCU effluent and/or SRU tailgas to flow backwards
down the combustion air line and escape from the blowers.
These devices will activate the TTO ESD to block the air line
before this can occur. The shutdown setpoint is 20% of normal
flow. Note that there are three independent transmitters and
2oo3 voting logic is used for the ESD (i.e., at least two
transmitters must show low-low flow) to avoid spurious "trips"
due to the malfunction of a single transmitter.
Loss of the fuel gas supply would cause the fuel gas pressure
to drop at the burner. This device will shut down the TTO
before flame instability creates the potential for an explosion.
The setpoint for these transmitters is 0.35 kg/cm2(g). Note that
there are three independent transmitters and 2oo3 voting logic
is used for the ESD.
Dual flame scanners are aimed to observe the flames from both
the pilot burner and the main gas burner. If the neither scanner
detects a flame (2oo2), a "flame failure" occurs and activates
the TTO ESD system. If only one scanner detects a flame
(1oo2), a malfunction alarm is activated in the DCS, but the
TTO ESD system is not activated. A third flame scanner,
A2-BY15758, is furnished with the pilot to detect its flame, but it
is used only to activate its status light (A2-GL15758) on the
These devices activate the TTO ESD system and shut down
the Thermal Oxidizer Burner if a temperature of 1000°C or
higher is measured in the Thermal Oxidizer. Temperatures
higher than this can overheat the refractory inside the Thermal
Oxidizer to the point that it weakens and fails, causing heat
damage to the Thermal Oxidizer shell. Excessive temperatures
in this furnace can also lead to damage of the tubes or casing
of the Thermal Oxidizer Waste Heat Boiler installed
downstream. Note that there are three independent
transmitters and 2oo3 voting logic is used for the ESD.
These devices activate the TTO ESD system and shut down
the Thermal Oxidizer Burner if the temperature of the
superheated steam leaving the second superheater pass of the
Thermal Oxidizer Waste Heat Boiler reaches 420°C. Steam
temperatures higher than this can lead to damage of the
superheater tubes, or damage the piping and equipment
downstream in the steam header and its users.
These devices prevent the water level from dropping too low in
the steam drum of the boiler. Hot combustion gas flows outside
the boiler tubes and will destroy these tubes if they are not
cooled by water boiling inside the tubes. The setpoint for these
devices will be specified by the boiler vendor. Note that there
are three independent transmitters and 2oo3 voting logic is
used for the ESD.
Once the pre-ignition steps have been completed and the BMS
gives a "PERMIT TO IGNITE" for the pilot burner in the Thermal
Oxidizer Burner (signaled by illuminating status indicator light
A2-AL15773 on the local TTO control panel), an ignition safety
interlock timer is started in the BMS. If an ignition attempt is not
made within 5 minutes, the TTO ESD system will be activated
to shut down the Thermal Oxidizer. This prevents a potentially
unsafe condition from persisting, where a leaking fuel gas valve
could cause an explosive mixture to form in the Thermal
Oxidizer, since the air flow is low at this point in the startup
procedure.
12.5.5.2 Effects
A Thermal Oxidizer shutdown, activated either manually or
automatically, has the following effects on the Tailgas Thermal
Oxidation system:
(1) Shuts off and depressurizes the main fuel gas supply by
closing block valves A2-NV15746 and A2-NV15748 and
opening vent valve A2-NV15747.
(2) Shuts off the pilot air supply by closing block valve
A2-NV15753.
(3) Shuts off and depressurizes the pilot gas supply by closing
block valves A2-NV15755 and A2-NV15757 and opening
vent valve A2-NV15756.
(5) Begins purging the pilot burner with air by opening block
valve A2-HV15782.
WARNING
IF EITHER SRU IS ON-LINE WHILE DRAINING SULFUR FROM THE
BOILER CASING, TGCU EFFLUENT OR SRU TAILGAS MAY BE
RELEASED TO THE SURROUNDINGS FROM THE DRAIN NOZZLE.
THIS PROCESS GAS CONTAINS TOXIC GASES (H2S AND
PERHAPS SO2). ALWAYS OBSERVE PROPER PROCEDURES
AND PRECAUTIONS WHEN USING THIS DRAIN CONNECTION.
THE "GENERAL SAFETY" SECTION OF THESE GUIDELINES
SHOULD BE CONSULTED IF THERE IS ANY DOUBT ABOUT HOW
TO WORK SAFELY WHEN H2S OR SO2 MAY BE PRESENT.
Too rapid heating or cooling can damage the refractory installed in the
Thermal Oxidizer. The Initial Cure and Normal Warmup schedules for the
refractory are provided by the refractory vendor. These schedules should
be adhered to quite closely.
CAUTION
Sudden drops in combustible content are most often caused by low H2S in
the TTO feed gas. This will usually only occur when SRU tailgas is being
routed directly to the TTO because the TGCU Unit is not in service.
Under these circumstances, if too much process air is fed to either SRU,
nearly all of the H2S will be consumed in the sulfur plant and the tailgas
from that SRU will contain only SO2. This will be indicated by high air
demand on the air demand controller in the SRU in question. However,
the sudden drop in the Thermal Oxidizer temperature is usually of no
consequence since the TTO feed contains very little H2S under these
circumstances, meaning that the potential loss of H2S oxidation efficiency
in the Thermal Oxidizer is not really of concern. The low furnace
temperature alarms in the DCS will alert the operator when this condition
occurs, as will the high air demand alarm on the air demand controller in
the DCS.
The more serious problem is when the combustible content of the TTO
feed gas suddenly increases and causes high temperature in the furnace.
The most common cause of this is high hydrocarbon content in the sulfur
plant feed stream(s). Hydrocarbons require 3-15 times more combustion
air per mole than H2S does. A sudden increase in the hydrocarbon
concentration of the acid gas (due to upsets in the upstream units) will
"starve" the sulfur plant(s) for air because the air demand controller(s)
cannot adjust the air:acid gas ratio enough to keep the SRU(s) on-ratio.
The available oxygen will burn the hydrocarbons preferentially over H2S,
with the result that insufficient H2S is reacted to form SO2. The SO2 that
does form will be completely consumed by the Claus reaction in the
furnace(s) and the catalyst beds, allowing large quantities of unreacted
H2S to leave the sulfur plant(s).
Even if the TGCU is in service at the time, H2S in these quantities will
overwhelm the capability of the TGCU solvent to absorb H2S. Thus,
WARNING
The procedure below describes how to switch from the "A" blower to the
"B" blower, for example. That is, the "A" blower is running to the TTO and
the "B" blower is not currently running. The procedure to switch from the
"B" blower to the "A" blower in the TTO is similar.
Make sure the SRUs, TGCU, and TTO are operating stably before
proceeding.
A. Confirm that the manual discharge valve on the off-line blower, the
"B" blower, is closed.
B. Start the "B" blower using its local start/stop control station.
C. Once the blower starts, slowly open its discharge valve, allowing time
for the air flow controller to adjust the air flow control valve to keep
the combustion air flow rate at the proper value.
D. Once the discharge valve on the "B" blower is fully open, slowly
close the discharge valve on the "A" blower, again allowing time for
air flow controller to adjust the air flow control valve.
E. Once the discharge valve on the "A" blower is fully closed, shut down
the "A" blower using its local start/stop control station.
F. The blower swap is now complete. Before leaving the area, visually
confirm that:
There are many qualified boiler and water treatment companies that can
advise the owner/operator on chemical treatment testing and controls. It
is recommended that only those companies that have local technicians
with extensive experience specifically in boiler water treatment be
selected to assist with Samsung Total Petrochemicals Co., Ltd.’s program.
The design details incorporated in the Thermal Oxidizer Waste Heat Boiler
have proven to be very reliable when combined with good operator
practice regarding water treatment. However, even properly designed
equipment can be severely damaged during a short period of operation if
the water treatment program is inadequate or improper.
Prior to using the intermittent blowdown valve, use the level controller in
the DCS to raise the water level in the boiler up to the high level alarm
point. Then open the intermittent blowdown valve until the level drops
back to the normal liquid level. Watch the boiler level in the sight glasses
throughout this operation to ensure that the level is not lost (which would
activate the TTO ESD and shut the Thermal Oxidizer down). Remember
to reset the level controller at the conclusion of this procedure.
D. Check all piping and equipment to be sure that all blinds have been
removed and that no valves are vented to atmosphere.
B. Use the quick-opening blowdown valve to lower the water level in the
boiler and check for proper operation of the level transmitters, the
low level alarms, and the low-low level shutdowns.
C. Fill the boiler with treated boiler feed water back up to the normal
liquid level.
E. Check all devices activated by the TTO ESD system to ensure that
they operate properly.
F. Check all relief valves to ensure that they are installed in the proper
locations and set for the correct relieving pressures.
12.7.3 Commissioning Fuel Gas, Pilot Gas, and I/A to the Process
The fuel gas, pilot gas (vaporized C4 LPG), and instrument air supplies to
the process side of the Thermal Oxidizer must be made ready for use
prior to starting up the Thermal Oxidizer using the procedures in these
guidelines. This requires blowing down each section of piping to ensure
that there are no liquids and/or construction debris in the headers and
supply lines. The procedure below can be used to make sure that these
gas utility systems are ready for service.
A. Select local manual control for the main fuel gas control valve by
switching the hand switch in the DCS to "local".
B. Set the manual fuel gas control on the local TTO control panel to 0%
output.
C. Confirm that the following fuel gas, pilot gas, and instrument air
valves are closed:
(1) The manual block valve(s) in the main fuel gas supply line.
(2) The manual block valve(s) in the main pilot gas supply line.
(3) The main fuel gas automated block valves, the fuel gas control
valve, and the block valve at the burner in the main fuel gas line
to the Thermal Oxidizer Burner.
(4) The manual block valve(s), and the two automated block valves
in the pilot gas supply line to the pilot.
(5) The block valve(s) in the main instrument air supply line.
(6) The manual block valves and the automated block valve in the
air supply line to the pilot.
(7) The manual block valve in the air supply line to the purges for
the burner instruments.
(8) The block valves in the purge lines to the burner instruments.
D. Confirm that all of the manual vent/drain valves in the main fuel gas,
pilot gas, pilot air, and purge air piping are closed.
E. If the orifice plate has already been installed in the fuel gas flow
meter, remove it for now.
F. Disconnect the fuel gas, pilot gas, and instrument air from the burner
system by performing the following steps:
(1) Unbolt the flanged connection at the burner in the main fuel gas
supply line.
(2) Disconnect the pilot gas supply tubing where it connects to the
pilot.
H. "Force" the PLC to open the following valves, then confirm they are
open:
(1) The automated block valves in the main fuel gas supply line to
the burner.
(2) The automated block valves in the pilot gas supply line to the
pilot.
(3) The automated block valve in the instrument air supply line to
the pilot.
I. "Force" the PLC to close the following valves, then confirm they are
closed:
(1) The automated vent valve on the main fuel gas supply line to
the burner.
(2) The automated vent valve on the pilot gas supply line to the
pilot.
J. "Crack" the manual block valve in the main fuel gas supply line
(upstream of the pressure regulator) and allow fuel gas to blow
through the piping until it is clear. Then close the block valve,
reinstall the main fuel gas supply pressure regulator, and reopen the
gate valve.
K. Using the pressure gauge and the vent valve downstream of the
main fuel gas supply regulator, adjust the main fuel gas regulator to
its specified setpoint.
L. Use the manual fuel gas controller on the local control panel to fully
open the control valve in the main fuel gas line, then use the
downstream drain valve to blow out this section of piping. Close the
drain valve when the piping is clear, then close the control valve.
M. Open the bypass valve around the main fuel gas control valve.
"Crack" the block valve at the burner and allow fuel gas to blow
through the piping until it is clear. Then close the block valve and
bypass valve.
N. "Crack" the block valve in the main pilot gas supply line to the pilot
(upstream of the pressure regulator) and allow pilot gas to blow
through the piping until it is clear. Then close the block valve,
reinstall the pilot gas supply pressure regulator, and reopen the block
valve.
O. Using the pressure gauge and the vent valve downstream of the pilot
gas supply regulator, adjust the regulator to its specified setpoint.
Q. "Crack" the block valve in the instrument air supply line to the pilot
and blow air through the piping until it is clear. Then close the block
valve, reinstall the pilot instrument air supply pressure regulator, and
reopen the block valve.
R. Using the pressure gauge and the vent valve downstream of the pilot
instrument air supply regulator, adjust the regulator to its specified
setpoint.
S. "Crack" the block valve downstream of the pilot air supply automated
block valve and allow instrument air to blow through the piping until it
is clear. Then close the block valve.
T. Remove the "forces" from the PLC and confirm that all of the
automated block valves close and all of the automated vent valves
open.
U. Close the block valve in the main fuel gas supply line (upstream of
the regulator), the block valve in the pilot gas supply to the pilot
(upstream of the regulator), and the block valve in the instrument air
supply to the pilot (upstream of the regulator) until the TTO is ready
for startup.
V. Reconnect the fuel gas, pilot gas, and instrument air to the burner
systems by performing the following steps:
(1) Bolt the flanged connection at the burner in the main fuel gas
supply line back together.
(2) Reinstall the pilot gas supply tubing where it connects to the
pilot.
(4) Reinstall the orifice plate in the fuel gas flow meter.
W. "Crack" the block valve in the instrument air supply line to the purge
rotameters (upstream of the purge pressure regulator) and blow air
through the piping until it is clear. Then close the block valve,
reinstall the purge instrument air supply pressure regulator, and
reopen the block valve.
X. Using the pressure gauge and the downstream drain valve, adjust
the purge instrument air regulator to its specified setpoint.
Y. Open the drain valve to blow out this section of piping until it is clear,
then close the drain valve.
Z. Each of the low pressure purges for the burner instruments has a
rotameter near where it connects to the process. Disconnect the
upstream fitting at each rotameter and open its upstream ball valve
briefly to blow any liquids or debris from the purge line. Reconnect
each rotameter, disconnect the fitting where each purge enters the
process, open its upstream ball valve, and open its needle valve
briefly to blow any liquids or debris from the purge line. Then
reconnect each purge to the process and open its needle valve to
place it in service.
CAUTION
B. Select local manual control for the air flow control valve by
switching the hand switch in the DCS to "local".
D. Select local manual control for the fuel gas control valve by
switching the hand switch in the DCS to "local".
N. Open the vent valves on the boiler to vent air from the steam
section.
O. Set the manual fuel gas control on the local TTO control panel
to 0% output.
Visually confirm that the main fuel gas valve, its bypass valve,
and the two main fuel gas shutdown valves are closed.
P. Set the manual air control on the local TTO control panel to 0%
output.
The "INLET OPEN" status light will flash until the valve has
moved to the proper position, then will be extinguished.
B. Verify that both of the local start/stop controls for the Thermal
Oxidizer Air Blower have their selector switches turned to the
"STOP" position.
C. Verify that the discharge valves are closed on both air blowers.
(1) Use the local start/stop control station to start the desired
blower.
For safety reasons, the PLC will not allow the light-off
sequence to proceed until these valves are proven
closed. Once the problem with the valves or their limit
switches has been corrected, the "LIMITS SATISFIED"
light will stop flashing and glow steadily, and the
light-off sequence can proceed.
G. Adjust the output of the local manual air control to open the air
flow control valve and allow a large air flow, 80% or more on the
flow indicator, to purge the furnace and downstream equipment
for 5 minutes. The "PURGE REQUIRED" light will be extinguished
and the "PURGE COMPLETE" light will be illuminated after about
40 seconds, but continue to purge the system for a full
5 minutes prior to this first time ignition attempt.
I. Adjust the output of the local manual air control to reduce the
air flow on the flow indicator to 10-20%. This will extinguish the
"PURGE COMPLETE" light and illuminate the "PERMIT TO IGNITE"
light, and the PLC will "enable" the ignition circuit.
(1) The air purge valve for the pilot burner is closed.
(3) The ignitor/pilot gas vent valve is closed and the block
valves are opened.
K. The air and pilot gas pressure regulators for the ignitor may
require some adjustment when first put in service before the
ignitor will light the pilot. However, once set properly, the ignitor
should ignite the pilot readily on subsequent startups. Refer to
the SRU Section of these guidelines for a suggested procedure
to adjust these regulators.
(4) The startup bypass in the PLC for the "flame failure" S/D is
disabled.
N. After the pilot is lit, use the local manual air control to increase
the air flow rate to about 50%, or as high a rate as can be
maintained without blowing the pilot out. When curing
refractory, it is best to keep the air flow as high as possible to
help distribute the heat more evenly and to heat the
downstream equipment more quickly.
O. The heat input from the pilot should be sufficient to reach the
first "hold" point in the refractory warmup schedule, 100-150°C.
If the temperature is too high, increase the air flow rate. If the
temperature is too low, decrease the air flow rate.
12.8.1.4 Igniting the Main Gas Burner, Refractory Cure-out and Warmup
When the firing rate needs to be increased to raise the furnace
temperature, the main gas burner can be placed in service. The
local manual control has control of the main fuel gas valve at this
time because the hand switch in the DCS is switched to "local". The
fuel gas flow rate can be monitored using the flow indicator on the
local TTO control panel and the flow indicator in the DCS.
A. Verify that the hand switch in the DCS is set to "local" to give
local manual control of the fuel gas control valve.
B. Confirm that the output from the manual fuel gas control on the
local TTO control panel is set to 0%, that the fuel gas control
valve and its bypass valve are closed, and that the two block
valves at the control station are both open.
C. Open the manual block valve in the main fuel gas line and the
manual block valve at the burner.
D. If the air flow rate is not at least 50%, use the local manual air
control to set the air flow at 50% as indicated by the flow
indicator.
(2) The main fuel gas automated block valves are opened.
(4) The "MAIN FUEL ON" light on the local TTO control panel is
illuminated.
NOTE: Be sure the air flow is above the low-low flow shutdown
point, about 20% on the flow indicator, or the TTO ESD
will be activated when the bypass timer expires and the
Thermal Oxidizer will shut down.
F. Use the manual fuel gas control on the local TTO control panel
to slowly open the fuel gas control valve until the burner lights
and has a stable flame. The "minimum fire" setting required for
this particular burner at the normal air flow will be determined
later.
H. As the firing rate increases, raise the air flow rate with the local
manual air control to 75%-80% as indicated by the flow
indicator.
I. Once the main fuel gas burner in the Thermal Oxidizer Burner
is operating smoothly, the pilot burner can be shut down and
retracted or extracted. For the initial startup of the Thermal
Oxidizer, this step should be performed after the "minimum fire"
setting for DCS the fuel gas control valve relay has been
determined.
(4) The air purge valve for the pilot burner is opened.
Verify that the air and pilot gas valves have moved to their
proper positions and that the pilot burner is being purged with
air as indicated by the rotameter.
(1) The manual block valves in the pilot gas supply to the
ignitor/pilot.
K. Loosen the packing gland on the pilot and retract or extract the
pilot assembly:
(c) Confirm that the pilot is still being purged with air as
indicated by the air flow rotameter.
(b) Close the block valve at the burner to isolate the pilot
from the furnace.
(c) Close the block valve in the purge air to the pilot
burner.
(3) Verify that the pilot burner mounting nozzle is still being
purged with air as indicated by the rotameter.
At this time, the steam pressure "toggle" switch in the DCS has
not yet been reset, so the steam leaving the superheater pass
is still being vented to atmosphere through the silencer.
S. Switch the combustion air flow control from the local TTO
control panel to the DCS as follows:
(2) Switch the air flow control hand switch from "local" to
"remote". The air flow controller now has control of the air
flow control valve, and will be controlling the air flow rate
with its last value as the setpoint.
(3) Slowly adjust the setpoint of the air flow controller to its
normal value.
The relay in the DCS will begin ramping down the output to the
steam blow-off valve. As the valve closes, the pressure in the
steam header will begin to increase until it is high enough to
open the check valve and the steam begins flowing to the
export header. Confirm that the blow-off valve closes fully.
(1) Adjust the output of the manual fuel gas flow control on the
local TTO control panel so that the reading displayed on
the hand indicator in the DCS matches the current output
from the temperature control.
(4) Raise the fuel gas flowrate back up slightly using the
manual fuel gas control until the flame is stable again.
(5) This is the actual "minimum fire" setting required for this
particular burner. Record the fuel gas flowrate on the flow
indicator in the DCS and the output on the manual fuel gas
control on the local TTO control panel.
(6) Use the manual fuel gas control to raise the fuel gas
flowrate back up to the value before starting this step.
Confirm that the temperature control is still in "automatic"
and its output is tracking the manual fuel gas control, then
switch the hand switch back to "remote" and adjust the
setpoint of the temperature control to its normal setpoint.
(2) After the limit switches prove this valve open, the TTO
bypass valve is closed.
WARNING
2. Place all steam heating systems in service. Check all steam traps
for proper operation, and use the vent valves to sweep
non-condensibles out of the steam spaces.
5. Confirm that the Thermal Oxidizer Waste Heat Boiler is filled with
water up to its normal liquid level.
B. Select local manual control for the air flow control valve by
switching the hand switch in the DCS to "local".
D. Select local manual control for the fuel gas control valve by
switching the hand switch in the DCS to "local".
G. Set the manual fuel gas control on the local TTO control panel
to 0% output.
Visually confirm that the main fuel gas valve and its bypass
valve are closed.
(b) Slide the pilot forward until it reaches the limit of the
retraction bar.
(a) Insert the pilot assembly into its packing gland and
open the block valve at the furnace.
(d) Open the block valve in the purge air to the pilot and
confirm that the pilot is now being purged with air.
(4) Verify that the pilot burner mounting nozzle is still being
purged with air.
The PLC will open the TTO bypass valve and close the TTO
inlet valve. Verify that the "BYPASS OPEN" light on the panel is
now illuminated and the "INLET OPEN" light on the panel is
extinguished.
B. Verify that the local start/stop controls for the blowers have their
selector switches turned to the "STOP" position.
C. Verify that the discharge valves are closed on both air blowers.
(1) Use the local start/stop control station to start the desired
blower.
For safety reasons, the PLC will not allow the light-off
sequence to proceed until these valves are proven
closed. Once the problem with the valves or their
(1) The manual block valves in the pilot gas to the ignitor/pilot.
H. Adjust the output of the local manual air control to open the air
flow control valve and allow a large air flow, 80% or more on the
flow indicator, to purge the furnace for 40 seconds and
extinguish the "PURGE REQUIRED" light. The "PURGE COMPLETE"
light will then be illuminated.
I. Adjust the output of the local manual air control to reduce the
air flow on the flow indicator to 10-20%. This will extinguish the
"PURGE COMPLETE" light and illuminate the "PERMIT TO IGNITE"
light.
NOTE: Remember that the ignition safety timer will shut down
the Thermal Oxidizer if an ignition attempt is not made
within 5 minutes of receiving the "PERMIT TO IGNITE".
M. Adjust the output of the local manual air control to increase the
air flow on the flow indicator to at least 50%.
B. If the air flow rate is not at least 50%, use the local manual air
control to set the air flow at 50% as indicated by the flow
indicator.
NOTE: Be sure the air flow is above the low-low flow shutdown
point, about 20% on the flow indicator, or the TTO ESD
will be activated when the bypass timer expires and the
Thermal Oxidizer will shut down. (This timer begins
running when the "MAIN FUEL START" push-button is
pressed, and has a 2 minute duration.)
D. Use the manual fuel gas control to increase the firing rate and
bring the Thermal Oxidizer back to its normal operating
temperature.
E. As the firing rate increases, raise the air flow rate with the local
manual air control to 75%-80% as indicated by the flow
indicator.
(1) The manual block valves in the pilot gas to the pilot.
(2) The manual block valves in the air supply to the pilot.
H. Loosen the packing gland on the pilot and retract or extract the
pilot assembly:
(c) Confirm that the pilot is still being purged with air.
(c) Close the block valve in the purge air to the pilot
burner.
(3) Verify that the pilot burner mounting nozzle is still being
purged with air.
K. Switch the combustion air flow control from the local TTO
control panel to the DCS as follows:
manual air control on the local TTO control panel, and its
setpoint is tracking its current value.
(2) Switch the air flow control hand switch from "local" to
"remote". The air flow controller now has control of the air
flow control valve, and will be controlling the air flow rate
with its last value as the setpoint.
(3) Slowly adjust the setpoint of the air flow controller to its
normal value.
The PLC will open the TTO inlet valve, then close the TTO
bypass valve. The "INLET OPEN" light will be illuminated, then the
"BYPASS OPEN" light will be extinguished as the valves move to
their new positions.
However, if you plan to enter any vessels for inspection or maintenance, then
more extensive and lengthy procedures must be followed to accomplish a
satisfactory shutdown and minimize the time required for performance of the
desired maintenance work. Section 12.9.2 that follows is an example of a
procedure for this circumstance.
One special circumstance that may exist during a shutdown is to have tube
leaks in the Thermal Oxidizer Waste Heat Boiler. This special case is discussed
in Section 12.9.3.
The TTO is affected directly and indirectly by shutdowns and outages that occur
in other systems both within the Sulfur Block and outside the battery limits. The
more important aspects of the effects these other systems can have on the
Thermal Oxidizer are discussed in Section 0.
Typical shutdown procedures are outlined and discussed in the sections that
follow for the more common cases. Your existing company procedures and
common sense operational judgment should be used to modify these
procedures as needed to serve the purpose of any given planned shutdown
situation.
A. If the SRUs and/or the TGCU are to be shut down also, shut down
the TGCU first using the appropriate procedures from Section 11.9
Then shutdown the SRUs using the appropriate procedures from
Section 9.9.
NOTE: If the SRUs are to remain in service while the TTO is shut
down, SRU tailgas or TGCU effluent (plus the Sulfur Surge
Tank sweep air and spent degassing air) will be flowing
through the Thermal Oxidizer. Since these gases contains
H2S (and possibly SO2), they should not be allowed to
escape to the surroundings except from the top of the
Thermal Oxidizer Vent Stack. The operating permit for
this plant may not allow venting un-oxidized process gases
for extended periods.
B. If the SRUs and the TGCU have been shut down, continue firing the
Thermal Oxidizer Burner with the main fuel gas burner for several
minutes to clear as much of the sulfur gases out of the system as
possible.
C. Use the "toggle" switch in the DCS or the push-button on the local
TTO control panel to activate the TTO ESD system.
This will open the Thermal Oxidizer Bypass valve and prove it open,
then close the Thermal Oxidizer Feed valve.
E. Close the manual block valves in the discharge lines of the Thermal
Oxidizer Air Blowers.
(1) The main fuel gas shutdown valves are closed and the vent
valve is open.
(2) The block valves in the main fuel gas line and pilot gas supply
line are closed.
(3) The automated block valve in the air supply to the ignitor/pilot,
and the automated block valves in the pilot gas supply to the
ignitor/pilot, are closed and the pilot gas vent valve is open.
(4) The Thermal Oxidizer Air Blowers are shut down and their
discharge valves are closed.
(1) Close the gate valve and the globe valve in the motive steam
supply line.
WARNING
E. Continue firing the Thermal Oxidizer Burner with the main fuel gas
burner for several minutes to clear as much of the sulfur gases out of
the system as possible.
NOTE: As the furnace temperature drops, the fuel gas flow rate
will become progressively lower. Once the fuel gas control
valve reaches its "minimum fire" position, it will not be
possible to drop the temperature any further.
(2) Visually confirm that the main fuel gas shutdown valves are
closed and the vent valve is open.
(3) Visually confirm that the automated block valves in the pilot gas
supply to the ignitor/pilot are closed and the vent valve is open.
(4) Close the gate valve in the main fuel gas supply line and the
gate valve at the burner.
(5) Switch the Startup/Run selector switch on the local TTO control
panel to "STARTUP".
(6) Switch the air flow control hand switch in the DCS to "local" so
that the manual air control on the local TTO control panel has
control of the air flow control valve.
(7) Start a Thermal Oxidizer Air Blower and open its discharge
valve.
(8) Press the "ESD RESET" push-button on the local TTO control
panel.
(9) Adjust the manual air control to send a large flow, 80% or more
on the combustion air flow line alarms, to the Thermal Oxidizer.
H. Allow the large flow of air to continue until the Thermal Oxidizer
reaches ambient temperature.
I. Once the Thermal Oxidizer is cool, use the "toggle" switch in the
DCS, or the push-button on the local TTO control panel to activate
the TTO ESD system.
J. Close the manual block valves in the discharge lines of the Thermal
Oxidizer Air Blowers.
(1) The main fuel gas shutdown valves are closed and the vent
valve is open.
(2) The block valves in the main fuel gas line and the pilot gas
supply line are closed.
(3) The automated block valve in the air supply to the ignitor/pilot
and the automated block valves in the pilot gas supply to the
ignitor/pilot are closed and the pilot gas vent valve is open.
(4) The Thermal Oxidizer Air Blowers are shut down and their
discharge valves are closed.
WARNING
CAUTION
3. If there is a large tube leak in the boiler, water may back-flow into
the hot Thermal Oxidizer and rapidly vaporize, possibly violently
enough to damage its refractory lining or create high pressure in
the Thermal Oxidizer.
A. Shut down the TGCU, shut down the SDU and shut off the Sulfur
Surge Tank Vent Ejectors. Shut down the SRUs.
D. Maintain a visible water level in the boiler. Water must remain in the
boiler until it is de-pressured and the Thermal Oxidizer has been
cooled to prevent overheating damage to the tubes.
F. The TTO is now ready to be isolated and made safe for entry.
When acid gas flow resumes to the SRU(s), SRU tailgas and/or
TGCU effluent will begin to flow once again to the Thermal Oxidizer.
The temperature control will automatically increase the fuel gas flow
as needed to increase the firing rate and continue oxidizing the gas
streams feeding the TTO.
When the TGCU warmup/bypass valve first opens, the pressure drop
through the TGCU will no longer be imposing back-pressure on the
SRUs. Depending on the magnitude of this change in back-pressure
(which is mainly determined by the unit throughput), there may be a
temporary "bobble" in the feed and air flow rates to the SRUs.
Although this will probably cause brief deviations from the proper
air:acid gas ratio in the SRUs, the "bobble" should not be large
enough to cause a "flame failure" shutdown in the SRUs. If so, the
SRUs will remain on-line with their tailgas flowing to the TTO.