Supervisory Operating Manual: UNIT NO.: 07 (Amine 2) Amine Regeneration Unit Cartagena Refinery Expansion Project

SUPERVISORY OPERATING MANUAL
UNIT NO.: 07 (Amine 2)

AMINE REGENERATION UNIT
FOR THE
CARTAGENA REFINERY
EXPANSION PROJECT
CB&I CONTRACT NO. 166004

Prepared By: Process - CB&I
Document No: 149-RP-PR35-0003.01
Information Class: Confidential Business Public
Revision Revision Revision Description Prepared Checked Approved
Number Date By: By: By:
0a 9-Dec-11 Issued for Information ELP AMC AMC

1 15-Mar-12 Issued for Information ELP AMC AMC
THIS DOCUMENT IS THE PROPERTY OF CHICAGO BRIDGE & IRON COMPANY ("CB&I"). IT MAY CONTAIN INFORMATION DESCRIBING
TECHNOLOGY OWNED BY CB&I AND DEEMED TO BE COMMERCIALLY SENSITIVE. IT IS TO BE USED ONLY IN CONNECTION WITH
WORK PERFORMED BY CB&I. REPRODUCTION IN WHOLE OR IN PART FOR ANY PURPOSE OTHER THAN WORK PERFORMED BY
CB&I IS FORBIDDEN EXCEPT BY EXPRESS WRITTEN PERMISSION OF CB&I. IT IS TO BE SAFEGUARDED AGAINST BOTH
DELIBERATE AND INADVERTENT DISCLOSURE TO ANY THIRD PARTY.
Document No.:
149-RP-PR35-0003.01
SUPERVISORY OPERATING
MANUAL
UNITS NO.: 07 Revision: 1
AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12
Page: Page 2 of 113
TABLE OF CONTENTS
1 INTRODUCTION 4
1.1 Confidential Note 4
1.2 Purpose of the Unit 4
1.3 Design Basis 5
1.4 Product Characteristics 6
1.5 Scope of Manual 6
2 PROCESS DESCRIPTION 7
2.1 Process Chemistry 7
2.2 Process Flow Description 7
3 MECHANICAL DESCRIPTION 10
3.1 Heat Transfer Equipment 10
3.2 Pressure Vessels 12
3.3 Rotating Equipment 17
3.4 Other 20
4 PREPARATION FOR STARTUP 21
4.1 Precommissioning Activities 21
4.2 Utility System Commissioning 22
4.3 Process Line Preparation 24
4.4 Cold Condensate Flush/Drain 26
4.5 Hot Condensate Flush/Drain 31
4.6 Prepare Amine 2 System for Weak Alkaline Solution Flush/Drain 32
4.7 Steam Out and Gas Blanketing 35
4.8 Prepare Amine Solvent Mixture 36
5 STARTUP 38
5.1 Amine Regeneration Check 38
5.2 Fill System and Establish Amine Solution Circulation 40
5.3 Start Operation of Heating and Cooling Systems 42
5.4 Introduce Sour Gas Feed to OSBL Absorbers 44
6 OPERATING GUIDELINES 46
6.1 Amine Temperatures 46
6.2 Amine Concentration 46
6.3 Lean/Rich Loadings 47
6.4 Steam Flow 47
6.5 Regenerator Pressure 48
6.6 Ammonia Control 48
Document No.:
149-RP-PR35-0003.01
MANUAL
Page: Page 3 of 113
7 TROUBLESHOOTING GUIDE 49
7.1 Foaming 49
7.2 Amine Solution Deterioration 51
7.3 Amine Solution Color Change 53
7.4 Amine Loading/Concentration 55
7.5 Fouling 56
8 SHUTDOWN 57
8.1 Cease Amine and Sour Hydrocarbon Gas Flows 57
8.2 Clean-Up Amine Inventory 58
8.3 Prepare for Maintenance and/or Amine Storage 60
9 MAINTENANCE 61
9.1 Replacing the Cartridge in the Rich Amine Pre-Filter, SU-F-2002 61
9.2 Replacing the Filter Media for SU-F-2003 and SU-F-2004 64
10 APPENDICES 65
10.1 Appendix 1 – Analytical Tests 65
10.2 Appendix 2 – Chemical Properties and Hazards (MSDS) 104
Document No.:
149-RP-PR35-0003.01
MANUAL
Page: Page 4 of 113
1 INTRODUCTION
1.1 CONFIDENTIAL NOTE

A considerable amount of CONFIDENTIAL information, which is the property of CB&I,
concerning the design, start-up and operation of Amine Regeneration Units is contained in this
manual. A SECRECY AGREEMENT in the contract between Reficar and CB&I, grants to
Reficar the use of this information only for the start-up, operation and maintenance of the Amine
Regeneration Units. Disclosure, reproduction or use of this manual for purposes other than the
start-up, operation and maintenance of the Amine Regeneration Units at Reficar’s Refineria de
Cartagena S. A. refinery in Cartagena, Colombia, Train 1, Train 2, and Amine 2 is a violation of
this agreement.
This manual provides the operating guidelines to assist the refinery to develop operating
procedures (based on both the refinery’s standard safe practices and experience) for the
Operations personnel in the start-up, operation and shutdown of the Amine Regeneration Unit. It
is emphasized that, though many critical and frequent problems are examined in this manual, not
all conceivable operating situations have been addressed in this guideline. Experience in the
operation of the units and thorough familiarity with the equipment and the process variables
involved should enable the Plant Operations staff to determine the action to be taken in any given
situation.
1.2 PURPOSE OF THE UNIT
Due to the staged nature of the FCCU revamp (Unit 002), Amine 2 will operate in three distinct
phases:
 Phase B – During a shutdown of the FCCU, tie-ins will be added for the addition of
equipment after Amine 2 is restarted. In addition, the trays in the Amine Regenerator
(SU-T-2) will be replaced to provide an increase in capacity for future operations. Amine
2 operations will remain essentially unchanged when the unit is restarted after this
turnaround. The only user of the regenerated lean amine will continue to be the existing
Amine Absorber (SU-T-1) which removes H2S (and CO2) from the FCCU Sponge Gas
stream.
 Phase B1 – While Amine 2 is operating, additional equipment will be installed (to be
described later). When this new equipment is ready for operation and when the new
Merox Unit (Unit 043) is ready for operation, the amine type will be changed from MEA
to DEA (probably accomplished by a short shutdown of Amine 2 for draining and
refilling). DEA can then be used to remove H 2S from the FCCU LPG liquid as well as
the FCCU Sponge Gas. The Absorber for the LPG is located in the new Merox unit.
Amine 2 will operate in this configuration until the DCU (Delayed Coker Unit, Unit 111) is
Document No.:
149-RP-PR35-0003.01
MANUAL
Page: Page 5 of 113
ready to receive lean amine. This could occur before the FCC 2013 Turnaround (Phase
D)
 Phase C/D – When the DCU is ready to receive DEA for treating the Coker LPG, the
FCCU Sponge Gas will be diverted to the new Fuel Gas Unit (Unit 133) and regenerated
lean amine will be routed to the DCU as well as to the Merox Unit. The DCU uses the
amine to remove H2S from the liquid LPG product and returns the rich amine to Amine 2
for regeneration.
The purpose of the Amine Regeneration Unit Amine 2 (Unit 07) is to regenerate rich
Diethanolamine solvent containing hydrogen sulfide (H2S) and carbon dioxide (CO2). The H2S
and CO2 are absorbed in various sweetening processes as described above. This rich amine is
regenerated by steam stripping the H 2S and CO2 out. The regenerated lean amine is cooled
and pumped to the absorbers. The H2S and CO2 stripped from the solution are sent as an amine
acid gas (AAG) stream to the Sulfur Recovery Units for further processing.
A depressurization step for the rich amine flashes hydrocarbon vapors with small amounts of
H2S and CO2. These vapors are routed to a compression system as follows:
 Phase B1 – FCCU Wet Gas Compressor
 Phase C/D – Liquid Jet Ejector compression system that increases the pressure of
several flash streams for final treating in the FGU (Unit 133).
Hydrocarbon liquids separated during the amine depressurization step are pumped out as slop
oil.
1.3 DESIGN BASIS
After completion of the revamp, Amine 2 is designed to regenerate, recirculate, filter and cool a
nominal 350 gpm of 25 wt% rich DEA solution for the sweetening operations. The following
table summarizes the rich amine feed stream arriving at the Rich Amine Flash Drum for each
operating case.
Case B1 Case C/D

SU-T-1 Merox Merox DCU
Flowrates, lb-mole/hr
CO2 12.1 2.8 0.01 0.03
H2O 3,400.9 2,298.7 2,388.9 4,058.0
H2S 35.7 20.5 28.1 12.4
DEA 195.8 131.9 136.8 232.2
Total 3,644.5 2,453.9 2,553.8 4,302.6
Temperature, °F 114 105 103 107
Pressure, psig 93 87 87 150
Document No.:
149-RP-PR35-0003.01
MANUAL
Page: Page 6 of 113
Case B is not included in the table above because the operation is not different than current
operation.
1.4 PRODUCT CHARACTERISTICS
The Amine Regeneration Unit is designed to regenerate the above solvent listed to an
approximate acid gas (H2S + CO2) loading of 0.02 mole of acid gas per mole of DEA.
1.5 SCOPE OF MANUAL
This manual is written primarily for the operation of the Amine 2 Regenerator (SU-T-2) and
associated equipment. The operation of the Merox Amine Absorber is covered as part of the
Merox Unit. The operation of the DCU Amine system is covered as part of the DCU Unit. The
operation of the existing Amine Absorber for the FCCU Sponge Gas (SU-T-1) with DEA (Phase
B1 only) is not significantly different than current operation. As with MEA, lean DEA entering
the column should be maintained 10 °F above the vapor entering the column to prevent
condensation of hydrocarbons. The design assumes that the lean DEA rate is essentially the
same as the current lean MEA rate to ensure proper functioning of the tower. The result is an
acid gas loading of approximately 0.25 moles acid gas per mole of DEA.
Document No.:
149-RP-PR35-0003.01
MANUAL
Page: Page 7 of 113
1 PROCESS DESCRIPTION
1.1 PROCESS CHEMISTRY

Function of the Amine 2 Regenerator (Unit 07) is to strip H2S and CO2 out of rich amine coming
from upstream amine absorbers to make lean amine. The resulting lean amine should be
approximately 25% diethanolamine (DEA) and 75% water by weight with small amounts of H2S
and CO2 residual. The lean amine is returned to the amine absorbers where it absorbs H2S and
CO2 from sour streams and becomes rich amine again.
In the absorbers, contacting H2S and CO2 with the lean DEA amine solution causes reactions
according to the following generalized equations:
H2S + R3N R3NH+ + HS -
DEA also reacts with the CO2 present in the sour gas.
CO2 + R3N + H2O R3NH+ + HCO3-
The regenerator reverses these reactions by steam stripping the absorbed H2S and CO2 from
the amine solution.
1.2 PROCESS FLOW DESCRIPTION

For Phase B1, the flow sequence and design operating conditions are depicted on process flow
diagrams 166000-07-B-1006-D and 166000-07-B-1007-D. The process flow diagrams for Phase
C/D have not yet been completed. However, the main effect is that the rich amine from SU-T-1
is replaced with rich amine from the DCU.
The rich amine streams are routed to the Rich Amine Flash Drum, SU-D-2007. Each steam
contains a backpressure controller to minimize flashing before entering the drum. The control
valves are as follows:
 Rich Amine from SU-T-1 (Phase B1 only) – The level control valve (LV-0104) for SU-T-1
serves as the backpressure controller
 Rich Amine from the DCU (Phase C/D) – Since SU-T-1 is out of service, the level control
valve for SU-T-1 will be retagged as PV-0153 and used as a backpressure control valve for
the DCU rich amine. The amine flow rates are similar for these two services
 Rich Amine from the Merox Unit (Phase B1/C/D) – This stream is fitted with a separate
backpressure control valve (PV-0155).
After flowing through the backpressure control valves, the two amine streams are combined and
enter the Rich Amine Flash Drum through a single nozzle. Light hydrocarbon vapor is flashed and
routed to compression. For some time after the initial startup, the flashed gases will be routed to
the FCCU Wet Gas Compressor, and flash drum operating pressure is estimated to be 22 psig.
Document No.:
149-RP-PR35-0003.01
MANUAL
Page: Page 8 of 113
After installation of a liquid jet ejector compression system for several flashed streams (new
sulfur block), the flash gases will be diverted from the Wet Gas compressor and the Rich Amine
Flash Drum will operate at approximately 7 psig. The new compression system will be
available prior to the FCCU 2013 Turnaround (Phase D). Any liquid hydrocarbon present in the
flash drum forms a layer on top of the amine solution and flows over the hydrocarbon weir into
the hydrocarbon separation bucket. The collected liquid hydrocarbon is routed to slop oil (GZ-
D-1204) on manual control.
After a majority of the hydrocarbon is removed, the rich amine is pumped from a separate
compartment in the flash drum by the Rich Amine Pumps, SU-P-2011 A/B/C (two operating, one
spare). Amine level is controlled automatically using a control valve at the Amine Regenerator
Inlet (LV-122). From the Rich Amine Pumps, the flow is routed to the Rich Amine Pre-Filter,
SU-F-2002. The pre-filter is a full flow filter providing continuous filtering to remove solids in the
rich amine. 30% of the rich amine is then split through the Rich Amine Charcoal Filter, SU-F-
2003, where dissolved hydrocarbon and some soluble impurities are absorbed. Following that,
the Rich Amine Post Filter, SU-F-2004, catches fine carbon to prevent foaming in the Amine
Regenerator. All of the rich amine then flows to the Lean / Rich Amine Exchanger, SU-E-1
(existing), where it is heated to approximately 165 F by the lean amine stream leaving the
bottom of the Amine Regenerator, SU-T-2 (existing).
Since the Rich Amine Pre-Filter does not have a spare, all filters will be bypassed when this
filter is cleaned. As a result, every effort should be made to clean the filter as quickly as
possible, and should not take longer than a shift. Cleaning may be required as often as once a
shift after the initial startup, but the cleaning frequency should quickly decline to no more than
once per week. A single bypass is provided for simultaneous on-stream servicing of the Rich
Amine Charcoal Filter and the Rich Amine Post Filter.
The rich amine stream enters the Amine Regenerator on the third tray from the top. In the
regenerator, the H2S and any CO2 are stripped out from the rich amine stream by hot vapors
generated in the Regenerator Reboiler, SU-E-2 (existing). The overhead vapor at 211 F enters
the Regenerator Overhead Cooler, SU-E-4 (existing), where the stream is cooled to 140F. The
condensed liquid is separated from the acid gas in the Acid Gas KO Drum, SU-D-2 (existing). The
condensed liquid is then pumped to the top of the regenerator as reflux by the Regenerator Reflux
Pump / Spare, SU-P-2 A/B (existing). Make-up water is provided by injecting steam from the
inlet of the Regenerator Reboiler (SU-E-2) into the reboiler return line via FI-111.
The acid gas from the regenerator overhead drum is sent to a liquid jet ejector system for
compression. The acid gas is routed to a liquid jet ejector, SU-J-2002. A high pressure (1240
psig) amine stream is also routed to the ejector. The high velocity generated by depressuring
the amine stream is used to entrain the acid and compress it. The mixture from the ejector is
routed to the Liquid Ejector KO Drum (SU-D-2008). The liquid from the drum is cooled (SU-E-
2009), pumped (SU-P-2009 A/B, operating/spare) and recycled to the ejector. Lean amine is
Document No.:
149-RP-PR35-0003.01
MANUAL
Page: Page 9 of 113
continuously added to the recycle loop using manual control, and rich amine is withdrawn to the
Amine Regenerator automatically using the drum level control valve (LV-0125). The acid gas
from the drum is routed to a sulfur plant (the existing sulfur plant after Phase B1 startup and
then to the new sulfur plant when it is available).
The purpose of the Liquid Jet Ejector compression system is to reduce the Amine Regenerator
pressure, thus reducing the temperature of the amine at the bottom of the tower. The
compression system reduces the tower overhead pressure to 5 psig, and the resulting amine
temperature at the bottom is 239 °F which minimizes amine degradation. Amine temperatures
up to approximately 260 °F are typically considered acceptable, but lower temperatures produce
less amine degradation.
The lean amine stream leaves from the bottom of the regenerator at 239 F by gravity flow into the
shell side of the Lean / Rich Amine Heat Exchanger, SU-E-1 (existing), where it is cooled to 191 F
by the rich amine stream feeding the regenerator. At this point, the flow of the lean amine depends
on the phase of construction as follows:
 Phase B1 – The lean amine is split into two streams. One stream is routed to the existing
Lean Amine Pump / Spare, SU-P-1 A/B (existing), followed by cooling and then enters the
FCCU Sponge Gas Absorber. The other stream is routed to the new Lean Amine
Circulation Pumps, SU-P-2006 A/B/C (only one required for Phase B1). After cooling in the
new Lean Amine Cooler, SU-E-2008 A/B, this stream is routed to the Merox unit.
 Phase C/D – As soon as the DCU is ready to receive lean amine, all the lean amine will be
routed to the new Lean Amine Pumps, SU-P-2006 A/B/C (2 operating, 1 spare), the new
lean amine coolers and then routed to both the Merox and DCU units.
Amine make-up will continue to be the same as present, except that DEA will be used. All new
drains are routed to the existing Amine Drain Drum, SU-D-4, which is reused in its current
service.
Document No.:
149-RP-PR35-0003.01
MANUAL
Page: Page 10 of 113
2 MECHANICAL DESCRIPTION (NEW EQUIPMENT ONLY)
3.1 HEAT TRANSFER EQUIPMENT
3.1.1 SU-E-2008 A/B LEAN AMINE COOLER
3.1.1.1 Principle Reference Drawings
P&ID: 4-07-EB-003 Sheet 4
3.1.1.2 Purpose
Cools lean amine before routing to users
3.1.1.3 Design Data
Design duty: 10.6 MM BTU/hr plus 10%

Heating Surface: 2104 ft2 per shell
Configuration: 2 shells in parallel
Design: Tubeside: 385 psig @ 300 °F
Shellside: 495 psig @ 400 °F
Materials: Tubes: SA-179-Killed
Channel: SA-516-70N
Shell: SA-516-70N Killed
PWHT: Shellside
3.1.1.4 Operating Conditions
Tube (Cooling Water): Inlet: 70 psig @ 90 °F

Outlet: 66 psig @ 103 °F
Shell (Lean Amine): Inlet: 327 psig @ 176 °F
Document No.:
149-RP-PR35-0003.01
MANUAL
3.1.2 SU-E-2009 LIQUID EJECTOR MOTIVE LIQUID COOLER
3.1.2.2 Purpose
Cools the rich amine recycle used as motive liquid for the Liquid Jet Ejector compression
system
3.1.2.3 Design Data
Design duty: 0.9 MM BTU/hr plus 10%

Heating Surface: 1,134 ft2
Configuration: 1 shell
Design: Tubeside: 120 psig @ 300°F
Shellside: 95 psig @ 250 °F
Materials: Tubes: SA-249-TP304L
Channel: SA-106-B
Shell SA-333-6N
PWHT: Shellside
Tube (Cooling Water): Inlet: 70 psig @ 90 °F

Shell (Rich Amine): Inlet: 44 psig @ 108 °F
Outlet: 41.5 psig @ 99 °F
Document No.:
149-RP-PR35-0003.01
MANUAL
3.2 PRESSURE VESSELS
3.2.1 SU-D-2007 RICH AMINE FLASH DRUM
3.2.1.2. Purpose
The Rich Amine Flash Drum operates at reduced pressure allowing volatile
hydrocarbons to flash out, reducing the potential for foaming in the Amine Regenerator.
In addition, the extended liquid residence time separates liquid hydrocarbons from the
rich amine solvent. Decanting the liquid hydrocarbons also reduces the potential for
foaming in the Amine Regenerator.
3.2.1.3 Design Data
Size: 10 feet Dia. x 36 feet T/T (horizontal)

Design: 75 psig @ 400°F / FV @ 400°F
Code: ASME Section VIII, Div. I
PWHT: Yes
Insulation: None
Material: Carbon Steel - HIC resistant

Liquid Inlet: 22 psig @ 111 °F Phase B1
7 psig @ 106 °F Phase C/D
3.2.1.5 Other
Internals:
 Equipped with two internal baffles which divide the drum into
three sections
 The hydrocarbon overflows the first baffle to skim hydrocarbon
off the rich amine into the hydrocarbon section.
 The rich amine underflows the hydrocarbon section and
overflows the second baffle into the hydrocarbon-free amine
section.
 One Inlet Stilling Well
 Three Vortex Breakers
Document No.:
149-RP-PR35-0003.01
MANUAL
3.2.2 SU-D-2008 LIQUID JET EJECTOR KO DRUM
3.2.2.2 Purpose
Collects and separates two phase mixture exiting the Liquid Jet Ejector. Acid gas is
routed to the sulfur plant and liquid amine is recycled to the ejector.
3.2.2.3 Design Data
Size: 6 feet Dia. x 15 feet T/T (horizontal)

Design: 150 psig @ 400°F / FV @ 400°F
PWHT: Yes
Insulation: None
Material: Carbon Steel - HIC resistant
Mixed Phase Inlet: 25 psig @ 149°F
3.2.2.5 Other
The drum internal includes an inlet elbow, wear plate and a vortex breaker
Document No.:
149-RP-PR35-0003.01
MANUAL
3.2.3 SU-F-2002 RICH AMINE PRE- FILTER
3.2.3.2 Purpose
The pre-filter removes particulate matter from the rich amine before carbon filtration.
3.2.3.3 Design Data
Size: 445 gpm, 2 feet diameter by 7 feet seam to seam (vertical)

Design: 230 psig @ 300°F / FV @ 300°F
PWHT: Yes
Insulation: None
Material: Carbon Steel - HIC Resistant, 304 SS Internals
Inlet: 74 psig @ 124 °F
3.2.3.5 Other
The filter is a cartridge type filter rated at 10 micron absolute. It takes 2 psi pressure drop
at clean and 10 psi at fouled conditions.
Document No.:
149-RP-PR35-0003.01
MANUAL
3.2.4 SU-F-2003 RICH AMINE CHARCOAL FILTER
3.2.4.2 Purpose
The Charcoal Filter removes soluble hydrocarbons and some degradation products from
the rich amine.
3.2.4.3 Design Data
Size: 6 feet Dia. x 18 feet – 6 inch T/T (Vertical)

Design: 230 psig @ 300 °F / FV @ 300 °F
PWHT: Yes
Insulation: None
Material: Carbon Steel - HIC resistant, 304L SS Internals
Inlet: 58 psig @ 124 °F
3.2.4.5 Other
The vessel contains 14.5 feet bed of mesh carbon with bottom support and top bed
limiter required. It operates at pressure drop less than 2 psi clean and 10 psi fouled.
Document No.:
149-RP-PR35-0003.01
MANUAL
3.2.5 SU-F-2004 RICH AMINE POST FILTER
3.2.5.2 Purpose
The Rich Amine Post Filter removes carbon particulate matter from the rich amine after
carbon filtration.
3.2.5.3 Design Data
Size: 134 gpm, 8 inches diameter by 80 inches seam to seam (vertical)

Design: 230 psig @ 300 °F / FV @ 300°F
PWHT: Yes
Insulation: None
Material: Carbon Steel, HIC resistant, 304/316 SS Internals
Liquid Inlet: 64 psig @ 124 °F
3.2.5.5 Other
The filter is a cartridge type rated at 10 micron absolute. It takes 2 psi pressure drop at
clean conditions and 10 psi fouled.
Document No.:
149-RP-PR35-0003.01
MANUAL
3.3 ROTATING EQUIPMENT
3.3.1 SU-P-2006 A/B/C LEAN AMINE PUMPS (2 Operating / 1 Spare)
3.3.1.2 Purpose
The Lean Amine Pumps transfer the regenerated amine from the Amine
Regenerator to the amine users.
3.3.1.3 Design Data
Configuration: Centrifugal, Horizontal

Design Capacity: 180 gpm each
Temperature: 175 °F
Suction Pressure: 3 psig
Discharge Pressure: 348 psig
Differential: 345 psi
Driver: Electric Motor, 125 hp
Material Casing / Impeller: API, S-8
Flow Rate: 164 gpm each
3.3.1.5 Other
Only one pump is required during initial operations (Phase B1)
Document No.:
149-RP-PR35-0003.01
MANUAL
3.3.2 SU-P-2009 A/B LIQUID EJECTOR PUMP / SPARE
3.3.2.2 Purpose
The Liquid Ejector Pump circulates amine solution to the Acid Gas Liquid Jet
Ejector, SU-J-2002, to provide the motive force for compressing the Amine
Regenerator Overhead.
3.3.2.3 Design Data
Configuration: Centrifugal
Design Capacity: 248 gpm
Temperature: 99 °F
Driver: Electric Motor
Material Casing / Impeller: API, A-8 NACE
Flow Rate: 225 gpm
Document No.:
149-RP-PR35-0003.01
MANUAL
3.3.3 SU-P-2011 A/B/C RICH AMINE PUMPS / SPARE (2 Operating, 1 Spare)
3.3.3.2 Purpose
The Rich Amine Pump moves rich amine from the Rich Amine Flash Drum
through the Rich Amine Filters, Lean / Rich Amine Exchanger, and into the
Amine Regenerator.
3.3.3.3 Design Data
Configuration: Centrifugal, Vertical

Design Capacity: 173 gpm each
Temperature: 106 °F
Driver: Electric Motor, 20 hp
Material Casing / Impeller: API, A-8 NACE
Flow Rate: 157 gpm each
Document No.:
149-RP-PR35-0003.01
MANUAL
3.4 OTHER
3.4.1 SU-J-2002 ACID GAS LIQUID JET EJECTOR
3.4.1.2 Purpose
The Acid Gas Liquid Jet Ejector uses a high pressure recirculating amine stream
to compress the acid gas from the Amine Regenerator
3.4.1.3 Design Data
Operating Pressures: Motive Fluid Inlet 1242 psig

Acid Gas Inlet 1 psig
Discharge 28 psig (35 psig max)
Motive Liquid Flow: 225 gpm
Acid Gas Flow: 2,543 lb/hr
Design Pressure: Motive Fluid Inlet: 1600 psig / FV
Body/Tail 150 psig
Design Temperature: 300 °F
Code: ASME Sec VIII, Div 1
PWHT: Yes
Insulation: None
Material: KCS with 316L SS Throat/Nozzle
Document No.:
149-RP-PR35-0003.01
MANUAL
4. PREPARATION FOR STARTUP
This section covers the activities that should be completed prior to the Amine Regeneration Unit
startup. The following steps are recommended for initial startup preparation:
 Step 4.1: Pre-commissioning Activities

 Step 4.2: Utility System Commissioning
 Step 4.3: Process Line Preparation
 Step 4.4: Cold Condensate Flush/Drain
 Step 4.5: Hot Condensate Flush/Drain
 Step 4.6: Prepare Amine Regeneration System for Weak Alkaline Solution
Flush/Drain
 Step 4.7: Steam-Out and Gas Blanketing
 Step 4.8: Prepare Amine Solution
Guidelines for these steps are given below. These activities are in addition to standard plant
safety and operating procedures for startup preparation. Appropriate portions of these
procedures should be repeated prior to subsequent startups after any unit repair, alteration, or
replacement has been made. For additional information on the upstream amine
scrubber/absorbers, contact the appropriate unit supervisor.
4.1 PRECOMMISSIONING ACTIVITIES
4.1.1 Hydrostatic and Pneumatic Testing
It is necessary that all new equipment / piping be subjected to a hydrostatic or pneumatic

pressure test. The design pressure of the equipment / piping will dictate which of these tests
will be conducted. Pressure testing is normally considered to be part of the construction efforts;
however, it is recommended that the test records are thoroughly reviewed to ensure that all
work has been completed and all deficiencies corrected prior to the commencement of any pre-
commissioning or commissioning activities.
4.1.2 Pre-Commissioning Walk Through
Prior to the commencement of any pre-commissioning activities, it is recommended that a

readiness review of the entire facility be conducted. The review should consist of, but is
certainly not limited to, the following steps:
a) Flow Plans Check
Document No.:
149-RP-PR35-0003.01
MANUAL
The flow plan check should consist of, but not limited to, the following:
 Verify that the routing of the process and utility piping conforms to the desired
process flow.
 Verify check valve orientations.
 Verify globe valve orientations.
 Verify that all instrumentation is properly installed.
 Verify that all steam tracing and insulation is installed where it is required.
 Verify that spectacle blinds are installed at the appropriate locations (orientation
will addressed at time of startup).
 Verify that temporary strainers/permanent strainers are in place.
 Verify that all steam traps are properly installed.
b) Verification that piping supports and shoes are properly installed and anchored
or guided as required.
c) Verification that spring hangers are prepared for normal operation in accordance
with manufacturers recommendations (pins should not be removed until all hydrostatic/
pneumatic testing is completed).
d) Verification that expansion joints have not been over-stressed by cold springing
and are prepared for normal operation in accordance with manufacturers
recommendations.
e) Verification that equipment is properly grounded.
Notations of all deficiencies should be documented and resolved prior to the commencement of
any pre-commissioning or commissioning efforts.
4.2. UTILITY SYSTEM COMMISSIONING
4.2.1 Electrical System Preparation
All electrical equipment must be commissioned by qualified electrical personnel. All motors
should be test run uncoupled to verify the motor and the control circuitry before running any
coupled machinery. Also verification of motor rotation direction should be completed. Electrical
systems should be tested and brought on-line in accordance with approved plant procedures
incorporating the above items.
4.2.2 Plant Air System and Instrument Air System
Document No.:
149-RP-PR35-0003.01
MANUAL
It is important that all instrument air piping be blown clean before admitting dry instrument air
from the instrument air system. To clean and dry the air systems, disconnect the instrument
lead lines from the main distribution pipe work and allow air to blow through the open lines until
all traces of dirt and moisture disappear. Utility hose stations should also be blown to clear the
system. To achieve the best cleaning results, blow the air lines at the highest velocity possible
without bleeding down the refinery’s main air header system. During the cleaning operation,
check the air headers for leaks.
4.2.3 Pumped Process Condensate
Flush from each utility hose station to clean the lines and ensure no blockage exists in the
distribution system. Disconnect water lines to machinery and flush through until the lines are
clear. Open high point vents to bleed air.
4.2.4 Nitrogen System (Inert Gas)
After hydrostatic testing, connect an air line to the nitrogen header at the battery limit, and blow
all nitrogen lines clear of water and dirt at open connections in the process area. Also blow back
to the supply. This system should be dry and dust free before admitting nitrogen from storage
to purge the complete system.
4.2.5 Steam System
Remove or turn to open position blind flanges at ends of steam headers and blow the line out
thoroughly to remove dirt and scale. Slowly increase the steam pressure on the live steam
headers, making sure the valves connected to process vessels and lines are closed and the
bleeders are open. One by one, open the branch lines making sure that the bleeders are open
near the end and that the header inlet valves to drivers are closed (if applicable). Bring all lines
up to full steam pressure slowly after they have been thoroughly flushed. Commission all steam
traps. Steam tracing systems should be checked and blown free of scale. Check and clean all
strainers. All filters should be removed until after the lines have been blown or flushed. Steam
traps should be checked for scale. Check for proper expansion of all steam headers and steam
lines.
4.2.6 Drain System Preparation
Preparation of the utility systems, auxiliary systems, process piping systems, and process
equipment will involve a great deal of flushing with a variety of fluids. To avoid area flooding
during the pre-commissioning efforts, it is recommended that the drain systems are
commissioned as soon as it is practical.
a) Open Drain Systems

Document No.:
149-RP-PR35-0003.01
MANUAL
The only connection to the Oily Water Sewer (OWS) is a hub at the hydrocarbon section
of the Rich Amine Flash Drum (SU-D-2007). Prior to use, this hub should have an
ample amount of service water or condensate poured into it to fill the loop seal.
Otherwise, the only open drains in the amine area are storm drains. The catch basins
are equipped with seals to minimize the evolution of odorous, flammable, or toxic vapors
from the underground system. This system may be used to drain water with small
amounts of contaminants.
b) Closed Drain Systems
The closed drain system should be commissioned in accordance with the existing plant
procedures.
4.2.7 Temporary Condensate Supply Preparation
Large quantities of cold clean condensate will be needed to flush and clean this system. The
condensate will be needed early in this procedure.
a) At the earliest practical time, thoroughly clean the storage tank, and Sump Drum,
the condensate inlet lines to these tanks and the outlet lines through and including their
pumps discharge lines.
b) Flush these lines to the storm drain. Close these drains and begin filling the tank
and sump with condensate so it has time to cool to ambient temperatures for later use.
4.3 PROCESS LINE PREPARATION
Purpose: Removal of debris and foreign matter from the unit.
General Guidelines: • Make sure the process inlet and outlet lines are isolated from the
next process.
• Blow or flush the unit in a segmental manner.
• Continue to blow or flush through each segment until there is no
debris observed exiting the segment.
Recommended Procedure:
4.3.1 Prepare for process line flushing and blowing as follows:
a) Make sure all process and utility lines are isolated at the battery limits.
Document No.:
149-RP-PR35-0003.01
MANUAL
b) All measuring elements, orifice plates, restriction orifices, and all special fittings
that may be blocked by debris must be removed from lines.
c) All instruments should be positively isolated from the lines.
d) Where practical, “roll” or “drop-out” all control valves to prevent pitting of the
valve seats due to deposition of debris on the seat. Wherever possible, the line should
be flushed or blown before installation of the valve to save duplicating effort. This
requires coordination of construction and start-up activities.
e) Fully open all block valves in the lines to be flushed and blown, except those
valves that isolate equipment.
f) Remove flappers from all check valves.
Note: Lines upstream of heat exchangers should not be blown or flushed into the
exchanger. The piping should be disconnected and the exchanger flange covered with a
piece of sheet metal. After flushing or blowing clear of debris, the line can be
reconnected and air or water flushed through the exchanger to the next section. This
will prevent blocking of exchanger tubes with debris. Exchanger bypass lines should
also be flushed or blown.
Note: Most of the debris dislodged during the flushing and blowing out operation will
accumulate in knock-out drums and vessels, which will be manually cleaned at the end
of the operation. Allow air to vent through the largest vents available upstream of the
equipment being isolated. If necessary, remove a block valve from the line for venting.
It is essential to obtain the highest possible gas velocity in order to completely remove
the foreign matter that may have been accumulated during construction.
4.3.2 Flush or blow out a section of the unit until no more scale and debris are dislodged.
Then repeat the procedure on the next section of the unit.
Warning: It is essential that all fittings, manhole covers, etc, be securely fastened
during the blowing out procedure since only a very small pressure is required to hurl
sizeable objects through the air. In addition, small objects in a high velocity air stream
can cause severe injury to personnel and damage to the equipment. Personnel working
in and around the area should be advised of this danger and should be equipped with
the appropriate safety equipment (goggles, filter type breathing masks, etc.). Further, an
area should be roped off at each equipment exit point to prevent personnel from being
inadvertently exposed to the high velocity debris.
Document No.:
149-RP-PR35-0003.01
MANUAL
4.3.3 At the conclusion of air blowing or water flushing of a system, check carefully to see that
piping is properly realigned, temporary piping has been disconnected, temporary breaks
reconnected, control valves reinstalled, check valve flappers or cover plates replaced, orifice
plates installed, etc. Block valves or other valves not “rolled” or “dropped out” during blowing or
flushing should be checked for closure and removed as required for cleaning. If valve gates
have to be removed for lapping, mark the gate and valve body to prevent replacing the wrong
gate.
4.3.4 Prior to final bolting of cover plates on manways, inspect the interior of all vessels for
cleanliness and for correct installation of internals.
In essence, the following flushing is required only for new equipment or equipment that has
been modified. However, typical practice has shown that best results are obtained if the entire
system is flushed after a major revamp to include significant new equipment. Please note that
new absorbers OSBL of the Amine 2 Regeneration Unit will also require flushing which is
typically done at the same time. For relatively small additions, procedures can be modified
accordingly provided that a good flush can be obtained. Without a good flush, significant
foaming can expected during and after startup.
4.4 COLD CONDENSATE FLUSH / DRAIN
Purpose: Clean the entire amine circulation system using cold circulating condensate.
General Guidelines: • Fill vessels with cold condensate from the amine storage tank.
• Establish circulation through system.
• Monitor equipment levels to prevent overfilling vessels and ensure
adequate suction head to pumps.
• Maintain minimum flow through pumps to prevent cavitation.
• Open valves on ancillary lines to flush all lines and equipment
items as required.
• Monitor equipment pressures and use vents and pressure control
valves as required preventing over pressuring or pulling a
vacuum.
Note: Steam condensate is preferred for amine system cleaning due to its high purity.
Treated water may be used if condensate is not available, but this will increase amine
solution foaming potential since some water may remain in the system after draining.
Boiler feed water should not be used as the additives in boiler feed water can cause
foaming.
Document No.:
149-RP-PR35-0003.01
MANUAL
4.4.1 Verify the following conditions:
• Make sure the OSBL unit supervisors are aware of startup activity in the Amine 2
unit.
• Be sure to use all "Lock-out Tag-out" procedures required by the plant.
• Isolate those scrubber/absorbers that will be excluded from the startup at their
respective battery limit lean amine inlet and rich amine outlet. Install battery limit
temporary bypasses where required. Install temporary bypasses where required at
the extreme ends of the amine circulating headers.
• Verify the state of the entire lean amine supply and rich amine return headers
system.
• Filter elements are not installed in either of the Pre-Filter or the Post Filter.
• Carbon has not been loaded into the Charcoal Filter.
• Suction strainers are installed in the Rich and Lean Amine Pump suction lines.
4.4.2 Open the block valves on all appropriate vessel gauge glasses and level transmitters.
4.4.3 Close all equipment drain valves to sewers.
4.4.4 Position drain connection and position drain valves such that the underflow/overflow
weirs in the Rich Amine Flash Drum (SU-D-2007) are bypassed. This will facilitate filling this
drum.
4.4.5 Using air or nitrogen, establish approximately 50 psig pressure in the participating OSBL
absorbers. Since the absorber bottoms are pressured back to Amine 2, establishing some
pressure allows circulation of wash solution to the absorbers and back to the Rich Amine Flash
Drum (SU-D-2007).
CAUTIONS:
 Do not use fuel gas for pressurization as the rest of the Amine 2 loop has
not been oxygen freed at this time.
 Existing pressure regulators for the OSBL absorbers must be used with
caution if air is used. If the stream leaving the absorber is routed to a
system containing hydrocarbon, the presence of air is undesirable.
 If available, temporary pressure regulators can be used to control pressure.
Otherwise, close attention by operating personnel will be necessary to
prevent either overpressure or pulling a vacuum.
 Avoid blowing relief valves to the flare if air is used for pressurization.
NOTE: For purpose of this procedure, it is assumed that the existing Amine
Absorber (SU-T-1) and the new Merox Amine Absorber (43-D-3201) will be
Document No.:
149-RP-PR35-0003.01
MANUAL
participating “OSBL” absorbers. While washing the existing Amine Absorber is not
necessary, it serves as a useful path to inventory the Amine 2 unit. During the 2013
FCC Turnaround, a new line will be added to route the discharge of the Amine
Transfer Pump (SU-P-5) directly to the Rich Amine Flash Drum (SU-D-2007).
NOTE: If DEA is to be used to supply the Coker Amine equipment before the 2013
FCC Turnaround, the Coker Amine equipment will require washing from another
source. One possible alternative – use the connection to the new MDEA system(s)
and wash along with the ARU’s.
4.4.6 Open the top vents on the following pieces of equipment: Rich Amine Flash Drum (SU-
D-2007), Acid Gas KO Drum (SU-D-2), Pre-Filter (SU-F-2002), the Charcoal Filter (SU-F-2003),
the Post Filter (SU-F-2004), Amine Regenerator (SU-T-2), and Liquid Jet Ejector Drum (SU-D-
2008). For the Amine Drain Drum (SU-D-4), the bypass around PCV-122 should be opened.
Make sure that natural gas is not flowing into the Amine Drain Drum (SU-D-4) at this time.
Note: This allows the air in these vessels to vent to atmosphere as they are filled with
water. It also makes it easier to drain the water from the vessels when necessary.
4.4.7 Line up the Liquid Jet Ejector System as follows:

 Close and Block PV-114 on the vapor outlet from the Acid Gas KO Drum (SU-D-2)
o This eliminates the potential for vacuum conditions in the Amine Regenerator
when washing the Liquid Jet Ejector System
 Roll Out the 6” valve for vapor to the Liquid Jet Ejector (SU-J-2002).
o This allows the Ejector to “compress” air during washing
 Remove 6” blind on top connection Liquid Jet Ejector Drum (SU-D-2008)
o This provides an outlet for the air “compressed” by the Ejector. A temporary
pipe to divert the flow to a safe location is recommended.
 Close and Block PV-0104 on the vapor outlet for the Liquid Jet Ejector Drum
o This minimizes the amount of equipment exposed to the air pulled by the
Ejector
 Line up the cooling water lines to the Liquid Ejector Motive Fluid Cooler (SU-E-2009)
and place the exchanger in service
o This prevents overheating the Liquid Ejector Pumps (SU-P-2009 A/B) when
circulating the wash liquid
4.4.8 Confirm that condensate has been added to the Amine Storage Tank (SU-TK-1) as
described in Section 4.2.7. Note the level in the tank.
Document No.:
149-RP-PR35-0003.01
MANUAL
4.4.9 Line up valves for routing condensate from the Amine Storage Tank (SU-TK-1) to the
existing Amine Absorber (SU-T-1) using the Amine Transfer Pump (SU-P-5) and one of the
existing Lean Amine Pumps (SU-P-1 A or B).
4.4.10 Following normal plant procedures, start the Amine Transfer Pump (SU-P-5) and one of
the existing Lean Amine Pumps (SU-P-1 A or B) per normal plant procedures to begin filling the
bottom of the existing Amine Absorber (SU-T-1).
4.4.11 When a level appears in the bottom of the existing Amine Absorber (SU-T-1), open the
level control valve (LV-0104B) and begin routing condensate to the Rich Amine Flash Drum
(SU-D-2007). Commission LIC-0104 to maintain level in the existing Amine Absorber (SU-T-1)
4.4.12 When the Rich Amine Flash Drum (SU-D-2007) level is about 3/4 full, line up the valves
for flow through the Pre-Filter (SU-F-2002) and on into the Amine Regenerator (SU-T-2), but
bypassing the Charcoal Filter (SU-F-2003) and the Post Filter (SU-F-2004). Then start one of
the Rich Amine Pumps (SU-P-2011 A or B or C) per normal plant procedures. This will begin
filling the Pre-Filter with condensate. The vent must be closed after the Pre-Filter is full. After the
Pre-Filter is full, the regenerator trays and reboiler will begin filling with condensate.
4.4.13 As allowed by the level in the bottom of the Amine Regenerator (SU-T-2), line up all
valves to allow pumping from one of the Lean Amine Pumps (SU-P-2006 A or B or C) to the
Merox Amine Absorber (43-D-3201). Check that the min flow bypass is in operation. Then start
one of the Lean Amine Pumps (SU-P-2006 A or B or C) per normal plant procedures.
4.4.14 When a level appears in the bottom of the Merox Amine Absorber (43-D-3201), open the
level control valve (LV-004) to recycle condensate to the Rich Amine Flash Drum (SU-D-2007).
Commission LIC-004 to maintain level in the bottom of the Merox Amine Absorber.
4.4.15 As permitted by the level in the Rich Amine Flash Drum (SU-D-2007), start a second
Rich Amine Pump (SU-P-2011 A or B or C) per normal plant procedures.
4.4.16 After the Amine Regenerator (SU-T-2) level glass is about 3/4 full, line up condensate
recycle to existing Lean Amine Pump (SU-P-1 A or B) that is operating and shutdown the Amine
Transfer Pump, SU-P-5)
4.4.17 After system circulation is established, transfer from manual mode to automatic mode for
flow control of the Rich Amine Pumps (SU-P-2011 A-C, two pumps operating).
4.4.18 Open the 2” condensate valves to the Charcoal Filter (SU-F-2003) and the Post Filter
(SU-F-2004) to begin filling. Note that this condensate might be hot (180 °F or higher). Close
the vents and condensate valve when full then put these vessels into circulation.
Document No.:
149-RP-PR35-0003.01
MANUAL
4.1.19 Open the 1” globe valve used to add lean amine to the Jet Ejector KO Drum (SU-D-2008)
and begin filling the drum by back flowing through SU-E-2009.
4.4.20 When the Jet Ejector KO Drum level glass is about 3/4 full, start one of the Ejector
Motive Fluid Pumps (SU-P-2009 A or B) per normal plant procedures. Before starting the
pumps, confirm that the equipment is lined up as specified in 4.4.7.
4.4.21 After stopping the condensate flow from the Amine Storage Tank (SU-TK-1), make
another written note of this vessel level. The net difference from the level noted in step 4.4.8 is
the minimum approximate volume of the entire system that received this cold flush, and the
volume difference will later be very useful as it is slightly less than the volume of the entire
Amine 2 system when full.
4.4.22 Continue circulating within the Amine 2 system for several hours. While circulating, the
following items should be done:
• Check system for leaks.

• Switch pumps and check strainers frequently.
• Flush all small bore piping and instrument connections with circulating condensate.
• Check operation of flow and level instruments.
• Open equipment and valve bypasses for flushing.
Note: Continue to monitor the level in the regenerator and add condensate as required to
maintain a reasonable level.
4.4.23 Flush the Rich Amine Flash Drum’s hydrocarbon collection system with condensate,
leaving a water seal in the hydrocarbon section. Do this by slightly increasing the Rich Amine
Flash Drum level above the height of the slop oil baffle. Open drain valves and flush the
hydrocarbon line to the Oily Water Sewer hub. After the flush water coming out of the
hydrocarbon collection system becomes clear, block the hydrocarbon line and then lower the
Rich Amine Flash Drum to its normal operating level.
4.4.24 Any dirt or oils left in any part of the amine circulation circuit can later cause significant
regenerator operating problems. However, other scrubbers use the header piping outside the
Amine 2 battery limits and close coordination with responsible parties of those units will be
required. Preferably at this time during this startup, flush the OSBL lean and rich amine circuit
lines to all these outside units and back to Amine 2. Where possible flush clean all lean and rich
amine distribution piping to and from these scrubbers during an Amine 2 initial startup, or make
sure temporarily connected pump condensate washes are done on the header piping and within
the battery limits of the non-participating units.
Document No.:
149-RP-PR35-0003.01
MANUAL
Caution: These actions must flush clean the distribution piping to each available absorber
through and including the inlet flow controllers, the Absorber vessels, the outlet level controllers
and downstream piping. Make sure no less than these parts are flushed within each battery
limits of every amine user, before final connection with the Amine 2 header piping.
4.4.25 After circulating within the participating Amine 2 system for several hours, shut down all
pumps and drain all the dirty condensate into the storm water sewer and not the Amine 2 drain
system. Repeat this process again until the drained water is clean.
4.4.23 Begin refilling the Amine Storage Tank (SU-TK-1) with a fresh load of pumped
condensate.
4.5 HOT CONDENSATE FLUSH/DRAIN
Purpose: Clean the Amine 2 Unit using hot circulating condensate. This step will remove
dirt and some oils that the cold condensate flush was unable to remove.
General Guidelines: • Fill vessels with cold condensate as deemed safe per plant
procedures.
• Establish circulation of warm condensate by operating reboiler.
• Monitor equipment levels to prevent overfilling vessels and ensure
• Open valves on ancillary lines as required for flushing all lines and
equipment items.
valves as required preventing over pressuring or pulling a vacuum.
4.5.1 Fill the Amine 2 system with clean condensate and establish circulation as described
above in steps 4.4.1 through 4.4.22, excluding step 4.4.21.
4.5.2 Line up the cooling water and place the Lean Amine Coolers (SU-E-2008 A/B) into
service.
4.5.3 To prepare for condensing the overhead vapor generated by operation of the reboiler,
line up the cooling water and place the Regenerator Overhead Condenser (SU-E-4) in service.
Confirm the vents on the top of the Regenerator are still open to avoid pulling a vacuum.
Document No.:
149-RP-PR35-0003.01
MANUAL
4.5.4 Manually introduce steam to the Regenerator Reboiler (SU-E-2). The steam will heat the
condensate and begin generating steam in the regenerator reboiler. Use the steam flow
controller, FIC-110, to slowly increase the steam to maintain a Regenerator bottom temperature
between 140 and 150 F. Close the vents on the Amine Regenerator level gauges.
4.5.5 If condensed liquid begins to collect in the Regenerator Overhead Drum (SU-D-2), open
the liquid outlet block valve on the suction valve for one the Reflux Pumps (SU-P-2 A or B). Set
the Regenerator Overhead Drum Level Controller in manual control and open the Reflux flow
control valve LV-110. When a liquid level appears in the Regenerator Overhead Drum (SU-D-
2), start a Regenerator Reflux Pump (SU-P-2 A or B) per normal plant procedures to return the
accumulated condensate in the drum to the Amine Regenerator (SU-T-2). Since it is unlikely
that liquid will accumulate sufficiently to run the pump continuously, shut the pump down when
the drum is nearly empty. Repeat as necessary to maintain the drum level.
Note: Additional condensate may be required as the overhead system is filled. Add
condensate as described in the previous section to maintain a level in the Rich Amine
Flash Drum.
4.5.6 Circulate the heated condensate for 6-8 hours. While circulating, the following items
should be done:
• Check system for leaks.

• Switch pumps and check strainers frequently.
• Flush all small bore piping and instrument connections with hot circulating
condensate.
• Check operation of all flow and level instruments.
• Verify the operation of temperature measuring instruments.
• Monitor the fluid temperature to the pump suctions. Excessive temperatures may
cause cavitation.
4.5.7 Flush the hydrocarbon collection system with hot condensate, leaving a water seal in the
Rich Amine Flash Drum internal hydrocarbon bucket (follow procedures in section 4.4.23).
4.5.8 After circulating for 6-8 hours, slowly decrease the steam flow to the Regenerator
Reboiler (SU-E-2) to zero flow while continuing to circulate condensate. Monitor equipment
pressures and temperatures closely as the system cools.
Caution: The cooling vapors may cause a vacuum to be created in the regeneration
equipment. Open additional vents as required to prevent this from occurring.
4.5.9 Shut down the pumps, open vents and drain the condensate after the system has
cooled.
Document No.:
149-RP-PR35-0003.01
MANUAL
4.6 PREPARE AMINE 2 SYSTEM FOR WEAK ALKALINE SOLUTION FLUSH/DRAIN
Purpose: Degrease new equipment by circulating a weak alkaline solution through the new
equipment and piping. This will remove any trace amount of hydrocarbon material left in the
equipment/piping. If not removed, even trace amounts of hydrocarbon can cause foaming upon
startup of the unit. This step may be omitted if no new equipment or piping was altered since
the prior unit shutdown.
Note: If caustic solution (NaOH) is used, the temperature shall not exceed 180 deg F to
avoid potential caustic stress corrosion cracking of SS parts and potential caustic
embrittlement of carbon steel equipment.
General Guidelines
• Fill the system with weak alkaline solution using similar
procedures as filling with condensate.
• Establish levels in the participating absorbers, and regenerator
and then stop adding condensate.
• Monitor equipment levels to prevent overfilling vessels and
insure adequate suction head to pumps.
• Open valves on ancillary lines as required flushing all new lines
and equipment items.
valves as required preventing over pressuring or pulling a
vacuum.
• Circulate the weak solution through the system using the lean and
rich amine pumps.
• Stop and drain the entire system through local drains, then close
these drain valves.
• Refill and re-establish circulation.
• Confirm Regenerator Overhead Condenser (SU-E-4) is in service.
• Activate steam to the Amine Reboiler to heat the circulating fluid.
Maintain 140 to 150 F in the circulating solution
• Continue reboiler operation for four hours. Pumpout Regenerator
Overhead drum as necessary
• Shut down system and drain the system again.
• Dispose of weak alkaline solution properly.
• Any oils used during fabrication must be removed using an
alkaline wash. Use either an amine (0.5 wt %), or sodium
carbonate (Na2CO3) (0.3%), or sodium hydroxide
(NaOH) (0.3%) solution.
Document No.:
149-RP-PR35-0003.01
MANUAL
• If NaOH or Na2CO3 solution is used, then the system shall be

rinsed and flushed several times with condensate until the
Na salt content is < 200 wppm in the dumped condensate.
• Fill again with condensate, circulate and drain.
• Steam out the system, then put it under a gas purge until ready to
be charged with 25 wt% amine solution.
Any oils left in the OSBL amine piping circuit can cause significant regenerator operating
problems. Preferably during this startup procedure the OSBL piping and equipment for lean and
rich amine distribution header lines to and from the Amine Regeneration System including the
equipment inside these OSBL units should also be washed with the circulating solutions. If this
equipment is not “participating” in the startup, verify it has previously been cleaned and
degreased.
Document No.:
149-RP-PR35-0003.01
MANUAL
4.7 STEAM-OUT AND GAS BLANKETING
Purpose: Displace air in all the participating Amine Regeneration Unit using steam.
Maintain positive pressure on vessels and prevent air from entering the system as steam from
steam-out condenses. This is accomplished using the appropriate blanket gas.
Note: Typically, nitrogen is used to blanket the regenerator and reflux drum, and sweet
fuel gas is used to blanket any participating absorbers and the Rich Amine Flash
Drum.
General Guidelines: • Successively steam-out sections to displace air from the

front end(s).
• Monitor equipment pressures and use vents to prevent
over pressuring equipment or pulling a vacuum.
• Regulate vents and control valves to purge air from all
equipment items and lines.
• Blanket by sections to facilitate completing steps in rapid
sequence required to prevent vacuum formation.
• Monitor equipment pressures and introduce nitrogen or
fuel gas as required to prevent pulling a vacuum on
equipment as steam from steam-out condenses.
• Use caution when blanketing with nitrogen to prevent
dosing the flare with inert gas.
4.7.1 Divide the Amine 2 system into manageable sections for steaming and blanketing and
identify relevant isolation valves.
4.7.2 Verify that the vents on the appropriate OSBL scrubber/absorbers, Amine Regenerator
(SU-T-2), Rich Amine Flash Drum (SU-D-2007), and Regenerator Overhead Drum (SU-D-2) are
all open. Make sure all vessels have been drained of liquid.
4.7.3 Re-install the 6” valve for vapor to the Liquid Jet Ejector (SU-J-2002).
4.7.4 Verify that the Amine Acid Gas battery limits block valves (amine acid gas to the SRU)
are closed.
4.7.5 Systematically start steaming upstream of the Rich Amine Drum, at the furthest available
points away from Amine 2 in the amine distribution headers. Sequentially introduce steam to all
Amine 2 equipment through the steam out connections located on various pieces of inlet vapor
line headers and equipment.
Document No.:
149-RP-PR35-0003.01
MANUAL
4.7.6 Proceed forward through the entire system. Open high point vents to purge air.
4.7.7 Regulate vents and low point drains as required to purge all equipment and piping runs.
4.7.8 If not already prepared, make required connections for blanket gas.
Note: Monitor system pressure and open additional vents or throttle steam as required. Verify
that all equipment and piping is purged of air.
4.7.9 Continue steaming and blanketing according to standard plant procedures.
Caution: Be prepared to immediately begin gas blanketing steps when steam is

discontinued since condensing steam can create a vacuum in the equipment.
4.7.10 For one section at a time, complete the following:
• Isolate section by closing appropriate valves.

• Discontinue steam flow.
• Close vents.
• Introduce blanket gas as required to prevent a vacuum.
• Monitor equipment pressure and regulate blanket gas addition to maintain a positive
pressure on equipment.
• Drain any steam condensate from low point drains as the system cools.
• Continue monitoring pressures and adding blanket gas until system is cool (ambient
temperature).
4.7.11 Repeat step 4.7.10 for every successive section of the participating Amine 2 system.
4.8 PREPARE AMINE SOLVENT MIXTURE
Purpose: Prepare a 25 wt% DEA solution to charge the complete (all inclusive) Amine 2
system. Note that it will take approximately 29,000 gallons to charge the
complete Amine 2 system and an additional 4,000 gallons for the Merox Absorber
and associated piping. Since the Amine Make-Up Tank (SU-TK-1) capacity is
about 15,000 gallons, it will take two tank batches to just charge the Amine 2
system and another partial tank batch for the Merox system.
General Guidelines: • Add correct amount of condensate to the Amine Make-Up Tank
(SU-TK-1) for a batch of 25 wt% DEA.
• Add DEA while circulating liquid through the tank.
Document No.:
149-RP-PR35-0003.01
MANUAL
• After adding the correct amount of DEA, continue to circulate

liquid through the tank for 30 minutes.
• Check the DEA concentration to be sure it is about 25 wt%.
4.8.1 Calculate the amount of condensate required to dilute a batch of DEA. Be sure to remember
to add charge volume for the empty portions of the complete system that are not included in this
startup.
4.8.2 Open the valve in the pumped condensate line to the Amine Make-Up Tank (SU-TK-1) and
add the correct amount of condensate for a tank full of 25 wt% DEA.
4.8.3 Line up the Fresh Amine Charge Pump (SU-P-5) to take suction from the tank and
discharge back to the tank via the return line. Begin circulation by starting this pump.
4.8.4 Add DEA to the Amine Make-Up via provided Truck Connection (or drums if truck supply
is not available).
4.8.5 After all the DEA has been added to the Amine Make-Up Tank (SU-TK-1), continue to
circulate the tank contents for about 30 minutes. Check the DEA weight percent to be sure it is
about 25%. When the solution concentration is correctly established and the solution is of
uniform concentration, stop the circulation by closing the circulating valves and stopping the
Fresh Amine Charge Pump (SU-P-5).
Note: The mixed solvent in the tank is ready to be charged to the DEA circulating system in
accordance with the procedure described in the Start-Up section of this guideline. As the
system is being charged, it will be necessary to mix another batch of 25 wt% DEA as the tank
inventory is depleted. Any amine solvent not charged to the circulation system from the last
batch can be stored in the Amine Make-Up Tank (SU-TK-1).
Document No.:
149-RP-PR35-0003.01
MANUAL
5 STARTUP
After startup preparation activities are complete, the Amine 2 Unit is ready for startup. Startup
consists of establishing amine circulation through the upstream amine users (absorbers) and
regeneration unit, establishing normal operating parameters, and then introducing sour feeds to
the absorbers. Once the Amine 2 system is operating and treating sour feed streams, startup is
complete. The following steps are required for a startup:
Step 5.1: Amine 2 Unit Check

Step 5.2: Fill System and Establish Amine Solution Circulation
Step 5.3: Start Operation of Heating and Cooling Systems
Step 5.4: Introduce Sour Gas Feed to Absorbers
Guidelines for these steps are described in the following sections. Distribution headers of lean
amine and rich amine, and scrubber/absorbers are located outside of the battery limit and not
covered by this guideline.
Caution: The OSBL equipment and piping headers that can be associated with
Amine 2 can be extensive. This procedure depends upon starting at the
most forward equipment items and finishing with the very last item. For
safety and reliability reasons decide at this time the extent of the OSBL
and ISBL equipment that will “participate” in this startup. Do not add new
equipment into this procedure from here on.
For safety and reliability reasons, all Amine 2 equipment must participate
in this procedure.
5.1 AMINE REGENERATION CHECK
Purpose: Verification that the Amine 2 Unit is ready for startup.
General Guidelines:  Conduct a complete walk through to confirm the unit’s readiness
to startup.
 Document and resolve any deficiencies.
5.1.1 Verify that the Amine 2 DCS is activated.
Document No.:
149-RP-PR35-0003.01
MANUAL
5.1.2 Verify that the utility systems are commissioned, and all steam traps are functioning
properly.
5.1.3 Verify that the nitrogen system or equivalent gas blanketing supply has been
commissioned.
5.1.4 Verify that the instrument air system has been commissioned.
5.1.5 Verify that the Regenerator Overhead pressure controller, PC-114, is set in automatic
mode with the correct operating pressure set point.
NOTE: A blanket of appropriate non-condensible gas must be maintained to the

Regenerator Overhead until Acid Gas becomes available. This action prevents pulling
a vacuum on the Regenerator.
5.1.6 Verify that the Amine 2 Regenerator is routed to the Flare with PV-143 fully open.
NOTE: To avoid pulling a vacuum on the Amine Regenerator, overhead vapors

should be bypassed around the Liquid Jet Ejector System until after Acid Gas
becomes available.
5.1.7 Verify that the Rich Amine Flash Drum pressure, PI-0156, is indicating a reasonable
pressure (after 2013 Turnaround, approximately 7 psig – before the 2013 Turnaround
approximately 20 psig – 5 psig or lower if lined up to the flare).
5.1.8 Verify that the slop oil system is ready to receive slop oil from the Rich Amine Flash
Drum (SU-D-2007).
5.1.9 Verify that the existing Amine Absorber (SU-T-1) and the new Merox Amine Absorber
(43-D-3201) are ready to receive amine and that the return valves are lined up to recycle it to
the Rich Amine Flash Drum (SU-D-2007). Level controllers for the absorbers should be closed,
and the towers should be gas blanketed with suitable gas to allow unpumped flow recycle.
5.1.11 Verify that the solvent system has been cleaned, flushed, steamed-out, and the
vessels that contain amine during normal operation are holding a slight positive pressure using
nitrogen or other appropriate gas. Use standard plant procedures that fully accomplish what
Chapter 4 describes. This must be done to prepare for Startup.
Note: Check that all oxygen has been removed from the system. The solvent should not
come in contact with oxygen because oxygen will cause degradation of the DEA.
Document No.:
149-RP-PR35-0003.01
MANUAL
5.1.12 Verify that the internals have been installed in the Pre-Filter (SU-F-2002) and the Post
Filter (SU-F-2004).
5.1.13 Verify that the activated carbon has been loaded into the Charcoal Filter (SU-F-2003).
5.1.14 Verify that the steam is available for the Amine Regenerator Reboiler (SU-E-2).
5.1.15 Verify that Rich Amine Pumps (SU-P-2011 A-C), Lean Amine Pumps (SU-P-2006 A-
C), Existing Lean Amine Pumps (SU-P-1 A/B), Reflux Pumps (SU-P-2 A/B), Liquid Ejector
Pumps (SU-P-2009 A/B), Sump Pump (SU-P-3), and Amine Transfer Pump (SU-P-5) have all
been prepared for operation in accordance with manufacturer's and refinery procedures.
5.1.16 Verify that the Regenerator Overhead Condenser (SU-E-4) and the Lean Amine
Coolers (SU-E-2008 A/B and SU-E-3 A/B) have been prepared for operation in accordance with
manufacturer's recommendations and standard refinery procedures.
5.1.17 Verify that the process condensate system is commissioned and ready to receive
condensate from the Regenerator Reboiler (SU-E-2).
5.1.18 Verify that a tank batch of 25 wt% DEA solvent has been prepared and is currently
stored in the Amine Make-up Tank (SU-TK-1).
5.1.19 Verify that the amine acid gas flare system is commissioned and its pilot is currently lit.
5.1.20 Verify all the Lean Amine Headers and Rich Amine Headers are capable of handling
additional flow. Verify that the Rich Amine Flash Drum (SU-D-2007), Regenerator Overhead
Drum (SU-D-2), Reboiler Condensate Pot (SU-D-3), Amine Sump Drum (SU-D-4) and Amine
Regenerator (SU-T-2) have all been prepared for operation in accordance with this manual, any
manufacturer's procedures, and refinery procedures. If the OSBL scrubbers/absorbers (SU-T-1,
Merox, and/or Coker as applicable) are to be started-up, verify that they have been prepared for
operation in accordance with this manual, their unit operating manual, any manufacturer's
recommendations, and standard refinery procedures that apply.
5.1.21 Verify the Amine Make-Up Tank (SU-TK-1) has been prepared for operation in
accordance with this manual, any manufacturer's recommendations, and standard refinery
procedures.
5.2 FILL SYSTEM AND ESTABLISH AMINE SOLUTION CIRCULATION
Purpose: Fill the equipment and piping to normal operating levels with 25% DEA
solution, and establish amine solution flows.
Document No.:
149-RP-PR35-0003.01
MANUAL
General Guidelines:
 Monitor equipment liquid levels to prevent overfilling vessels and ensure
 Maintain minimum flow rates to pumps to prevent cavitation.
 Monitor system pressures and bleed any excess pressure to appropriate
destinations.
5.2.1 Position drain connections and position drain valves such that the underflow/overflow
weir of the Rich Amine Flash Drum (SU-D-2007) is bypassed by opening the forward and after
chamber drains. This will facilitate filling this drum.
5.2.2 Line up valves to transfer amine solution from the Amine Make-Up tank to the existing
Amine Absorber (SU-T-1).
5.2.3 Start flow to the existing Amine Absorber (SU-T-1) by adding amine solution from the
Amine Make-Up Tank (SU-TK-1), using the Amine Transfer Pump (SU-P-5) and the existing
Lean Amine Pumps (SU-P-1 A/B).
5.2.4 When the level in the bottom of the Amine Absorber (SU-T-1) is approximately 3/4 full,
commission the level controller (LIC-104) and begin routing amine to the Rich Amine Flash
Drum (SU-D-2007).
5.2.5 When the Rich Amine Flash Drum (SU-D-2007) level is about 3/4 full, start one of the
Rich Amine Pumps (SU-P-2011 A or B or C) per normal plant procedures (i.e., discharge valve
in appropriate position). This will put amine onto the regenerator trays and into the reboiler.
5.2.6 When the Amine Regenerator (SU-T-1) level glass is approximately 3/4 full, check that
the low flow bypass for the Lean Amine Pumps (SU-P-2006 A-C) is commissioned, and that the
discharge of the pumps is lined up to the Merox Absorber. Start one of the new Lean Amine
Pumps (SU-P-2006 A or B or C) per normal plant procedures. This will route amine to the
Merox Absorber.
NOTE: A second new Lean Amine Pump (SU-P-2006 A or B or C) is not required until
the Coker requires DEA for treating LPG.
5.2.7 When the level glass at the bottom of the Merox Amine Absorber (43-D-3201) is
approximately 3/4 full, commission the level controller (LIC-004) to return lean amine to the Rich
Amine Flash Drum (SU-D-2007).
Document No.:
149-RP-PR35-0003.01
MANUAL
5.2.8 As permitted by level in the Rich Amine Flash Drum (SU-D-2007), start a second Rich
Amine Pump (SU-P-2011 A or B or C) per normal plant procedures.
5.2.9 Open globe valve on lean amine line to the Liquid Ejector System and fill the Liquid
Ejector Drum approximately 3/4 full by backflowing through SU-E-2008. Close the globe valve.
NOTE: The Liquid Ejector Pumps (SU-P-2009 A/B) should not be started until acid gas
has reached the top of the Amine Regenerator (SU-T-2) in order to prevent pulling a
vacuum on the Amine Regenerator and associated equipment.
5.2.10 When the Amine Regenerator (SU-T-2) level glass is about 3/4 full, line up amine
recycle to existing Lean Amine Pump (SU-P-1 A or B) that is operating.
5.2.11 Stop amine addition to the Rich Amine Flash Drum and Amine Regenerator after normal
levels have been established in all the OSBL absorbers and the amine regeneration equipment.
5.2.12 Line up the hydrocarbon slop line from the Rich Amine Flash Drum (SU-D-2007).
Commission the associated level transmitter (LT-018). Manually drain any hydrocarbon that
appears as needed.
5.2.13 Close the forward chamber drain of the Rich Amine Flash Drum that is bypassing the
weir drain.
5.2.14 Continue circulating amine through the Amine 2 Unit and associated Amine Absorbers
and proceed to the next step.
5.3 START OPERATION OF HEATING AND COOLING SYSTEMS
Purpose: Put the heating and cooling equipment (Regenerator Reboiler, Regenerator
Overhead Condenser, Lean/Rich Exchanger and Lean Amine Coolers) in
service to establish circulating flows at operating temperatures.
General Guidelines:
 Monitor Regenerator Reboiler temperature to ensure amine
solution is not heated too rapidly.
 Maintain adequate cooling of amine solution to prevent pump
cavitation.
5.3.1 If not already completed, line up and commission cooling water to the Lean Amine
Coolers (SU-E-2008 A/B and the existing SU-E-3 A/B).
Document No.:
149-RP-PR35-0003.01
MANUAL
NOTE: As with MEA, the amine temperature to the existing Amine Absorber (SU-T-1)
must be maintained higher than the process gas temperature to the absorber to prevent
condensation of hydrocarbons that could produce foaming in the Amine Regenerator
(SU-T-2).
5.3.2 If not already completed, line up and commission cooling water to the Regenerator
Overhead Condenser (SU-E-4) so when steam is introduced into the reboiler, the condenser will
produce reflux.
Note: Until acid gas appears at the top of the regenerator, a suitable flow of non-
condensible gas must be maintained to prevent pulling a vacuum. At this point, the
vapor stream from the Regenerator Overhead Drum (SU-D-2) should be lined up to the
flare.
5.3.3 After commissioning the Steam Desuperheater (TIC-123), introduce steam to the
Regenerator Reboiler (SU-E-2). The steam will heat the amine solution as it passes through the
reboiler and begin generation of Amine Regenerator overhead vapors. Use the reboiler steam
flow controller, FIC-110 in automatic mode to control the flow of steam.
Caution: Do not heat the amine solution too rapidly as this could cause localized
overheating in the reboiler tubes and lead to corrosion.
5.3.4 Open the suction valve on the Amine Regenerator Reflux Pump (SU-P-2 A or B). When
a liquid level appears in the Regenerator Overhead Drum (SU-D-2), start one reflux pump per
normal plant procedures (i.e., discharge valve in appropriate position) to return this accumulated
liquid back to the Amine Regenerator (SU-T-2).
Note: Additional amine solution may be required as the overhead system is

filled. Add amine solution as described in the previous section to maintain an
appropriate level in the Amine Regenerator.
5.3.5 When permitted by level in the Amine Regenerator Overhead Drum (SU-D-2),
commission the level controller (LIC-110) to maintain level.
5.3.6 Adjust the reboiler steam flow controllers, FC-110 to approximately 12,000 lb/hr. This
should be sufficient to maintain level in the overhead drum and establish traffic in the
regenerator.
5.3.7 Set the set point of the Rich Amine Flash Drum level controller, LIC-0122, to its target
value.
Document No.:
149-RP-PR35-0003.01
MANUAL
5.3.8 After the lean amine flows are established to and from the absorbers, check the level
controls of each to make sure they are working properly.
5.3.9 Slowly increase the reboiler steam rate to 0.9 lb per gallon of circulating rich amine fed
to the regenerator.
5.4 INTRODUCE SOUR GAS FEED TO OSBL ABSORBERS
Purpose: Introduce sour feeds to the absorbers for removal of acid gas by the circulating
amine solution.
General Guidelines:  Verify that amine system flow rates, temperatures, and
pressures are operating at or near design values
before introducing sour feed.
 Review the treatment performance after the amine flow is
introduced.
 Advise upstream and downstream operations that
desulfurization is about to startup.
Recommended Procedures:
5.4.1 Check the strength of the solvent circulating in the system to make sure it is about 25 wt
% DEA.
5.4.2 Advise participating absorber units when Amine 2 is ready to receive rich amine. Advise
the Amine 2 supervisor that amine acid gas will soon be available.
5.4.3 The participating unit absorbers will now gradually introduce H2S containing streams to
the absorbers.
5.4.4 The amine solution leaving these absorbers is now called rich amine since it contains
absorbed H2S. As H2S is stripped out of the rich amine in the Amine Regenerator, the overhead
vapor becomes rich in H2S. At this point, the overhead vapor is still routed to the flare.
5.4.5 When the Amine Regenerator (SU-T-2) operation is stable, commission the overhead
controller (PIC-114) and stop the flow of non-condensible gas.
5.4.6 The Liquid Ejector System can now be put into service. Check that the Liquid Ejector
Drum (SU-D-2008) has an adequate level to start a Liquid Ejector Pump (SU-P-2009 A or B). If
not already done, line up and commission cooling water to the Liquid Ejector Motive Fluid
Cooler.
Document No.:
149-RP-PR35-0003.01
MANUAL
5.4.7 Open the block valves for vapor to and from the Liquid Ejector System. Leave the
bypass open until after the pump is started.
5.4.8 Start on Liquid Ejector Pump (SU-P-2009 A or B) per normal plant procedures. Close the
bypass valve for the Liquid Ejector System.
5.4.9 Set amine flow to the Liquid Ejector system using FI-0120 and the associated manual
globe valve.
5.4.10 Commission the level controller for the Liquid Ejector Drum (LIC-0125). It may be
necessary to backpressure the drum using PIC-0184 to ensure that the amine purge can return
to the Rich Amine Flash Drum (SU-D-2007) particularly before the FCC 2013 Turnaround when
the flash drum operates at higher pressure (gases routed to FCCU Wet Gas Compressor).
5.4.11 When the downstream sulfur plant is ready to receive acid gas, line up the valving
accordingly (existing Sulfur Plant before the FCC 2013 Turnaround and the new Sulfur Plant
afterwards).
5.4.12 Allow some time for the lean amine to equilibrate to a normal lean concentration, and
then perform absorber outlet gas composition analysis for each absorber. See Sections 6 and 7
for more information on fine tuning the system.
5.4.13 Review liquid levels in the Rich Amine Flash Drum and Amine Regenerator and add
additional solvent to attain normal levels in each of these vessels.
Document No.:
149-RP-PR35-0003.01
MANUAL
6 OPERATING GUIDELINES
Proper operation of the Amine 2 Unit is essential to meet the absorbers product specifications
for H2S removal. Proper startup, operation, and shutdown of the Amine 2 Unit are essential for
the safety of the operators, and to meet the Amine Regenerator bottoms product specifications.
Corrosion and DEA solution losses can be minimized by proper operation of the Amine 2 Unit.
Please refer to Process Description and Troubleshooting Guide below for additional information
relative to successful plant operations. The following operating conditions are discussed in this
section:
 Step 6.1: Amine Temperatures

 Step 6.2: Amine Concentration
 Step 6.3: Lean/Rich Loadings
 Step 6.4: Steam Flow
 Step 6.5: Regenerator Pressure
6.1 AMINE TEMPERATURES
Lean amine feed temperature to each amine absorber that treats a hydrocarbon rich gas stream
should be maintained at least 10ºF higher than the sour gas feed temperature to prevent
condensation of hydrocarbons in the amine leaving the absorber. Hydrocarbon in the rich
amine will cause operational problems in the Amine Regenerator. Hydrocarbon in the acid gas
to sulfur plant will result in potential sooting problems in the reaction furnace and carbon deposit
in the 1st catalyst bed.
The main control point of the rich amine temperature returning to the unit is the lean amine
temperature leaving the unit. The lean amine solution temperature is important to meet the
treated gas H2S specification at each absorber, and should be carefully controlled. In general,
the lower the lean amine temperature, the lower the H2S in the treated stream. However, vapor
absorbers require special attention as noted in the paragraph immediately above.
The temperature at the bottom of the Amine Regenerator should be maintained less than 260 F
to prevent excessive amine degradation. Temperatures lower than 250 F are ideal. The Liquid
Ejector system has been added to insure that regenerator temperatures remain low. If the
ejector system must be shutdown while the Amine 2 unit continues to operate, regenerator
bottoms temperatures should be watched closely.
6.2 AMINE CONCENTRATION
The design amine (DEA) concentration is 25% by weight. For most DEA plants the solvent
concentration can vary as much as 4% absolute and still operate successfully. However, if the
Document No.:
149-RP-PR35-0003.01
MANUAL
solvent concentration drops below 20%, efforts should be made to increase the solvent
concentration to a minimum of 20%, and preferably back to the design of 25%.
If necessary due to high sulfur contents of treated streams, the DEA content can potentially be
increased. However, 40 wt% is the maximum typically recommended. Higher DEA
concentrations are somewhat more difficult to regenerate. In addition, as the DEA
concentration increases beyond 40 wt%, the solution viscosity increases. Higher viscosity
results in reduced DEA absorber contact efficiency. This results in a reduction of H2S
absorption, potentially failing to meet the H2S specification of the treated absorber product
streams.
The water balance of the Amine Regeneration Unit depends upon the water contribution by
upstream absorbers. The design feed basis requires a nearly continuous flow of condensate
make-up.
There are several ways to increase or reduce the DEA concentration of the amine solution.
Please refer to, Troubleshooting Guide, for possible action to adjust the unit operations.
6.3 LEAN/RICH LOADINGS
The amine loading is defined as the amount of total acid gas (H2S + CO2) in either of the amine
streams (lean and/or rich) compared to the amount of amine present. Typically, these values
are expressed as moles of total acid gas per mole of amine. The design lean amine loading is
0.02 moles of total acid gas per mole of active DEA. The design, rich amine mole loading
depends on the treating service. For the existing vapor absorber (SU-T-1), the total acid gas
loading (H2S + CO2) should be maintained at approximately 0.25 per mole of active DEA.
Loadings up to approximately 0.35 are acceptable, but amine regeneration may be slightly more
difficult. The Merox Amine Absorber is designed for a total acid gas loading of 0.18. In general,
the maximum loading for liquid absorbers is less than vapor absorbers. The amine treating
system in the Coker is comprised of several steps, and the design total acid gas loading in the
rich amine return stream is 0.05. For best results, both the lean and rich DEA should be tested
daily by the plant laboratory.
If the lean DEA loading is too high it can be adjusted by 1) increasing the steam rate to the
reboiler, 2) increasing the lean DEA feed rate to the absorbers, and/or 3) increasing the DEA
concentration. There is no significant penalty for a lean loading less than 0.02 moles of total
acid gas (H2S + CO2) per mole of DEA.
6.4 STEAM FLOW
Since the acid gas loadings in the DEA are available infrequently, the operator needs a guide to
ensure that the DEA is being satisfactorily regenerated. One very good guide is the total steam
Document No.:
149-RP-PR35-0003.01
MANUAL
flow to the regenerator reboiler, as compared to solvent feed rate. The steam rate is controlled
as a ratio to the rich amine solution rate to the regenerator. The minimum steam rate for
successful regeneration should be 0.9 lb/gal amine solution.
6.5 REGENERATOR PRESSURE
The regenerator pressure governs the top and bottom temperature of the regenerator. The
design Regenerator Overhead Drum operating pressure is 3 psig, which essentially sets the
boiling point of the 25% (by weight) DEA solution. Therein, the tower bottoms (or reboiler
temperature) is approximately at 239ºF, as long as the DEA concentration is near 25%. Equally
important is the overhead gas temperature upstream of the overhead condenser, which is
designed to be 211ºF. Therefore, throughout the tower, there is only a 28ºF temperature
differential from the bottom to the top. However, these top and bottom temperatures are
important in relation to the efficiency of solvent regeneration. On the basis that the overhead
reflux drum pressure is maintained at 3 psig, these top and bottom vapor temperatures should
not generally deviate more than about 10%. That is, the reboiler temperature usually should not
be below 215ºF and the overhead vapor temperature should not fall below 190ºF. If either of
these items occurs, then the steam rate to the reboilers should be increased to raise either or
both of these vapor temperatures. However, it should be noted that once the solvent is boiling,
the actual operating pressure at the point the temperature is measured, sets the temperature.
6.6 AMMONIA CONTROL
Ammonia is not expected to be present in any of the treated streams associated with Amine 2.
However, process upsets could result in some ammonia in the rich amine stream to Amine 2. If
this happens, periodic 10-25% regenerator reflux purging may be required to minimize ammonia
salt plugging and corrosion issues.
Document No.:
149-RP-PR35-0003.01
MANUAL
7 TROUBLESHOOTING GUIDE
7.1 FOAMING
Possible Causes Action to be Taken
7.1.1 Entrained  Prevent liquid hydrocarbon from entering the plant.

hydrocarbon  Check amine absorber inlet temperature. Maintain amine temperature
10°F above the feed gas. Applies to vapor absorbers only.
 Do not feed rich amine from the contactors directly to the regenerator.
Rich amine should be routed through the flash drum before processing in
the regenerator.
 Lower the set pressure on the rich amine flash drum to flash more light
hydrocarbons from amine solution.
 Check and maintain the amine level in the rich amine flash drum to
skim liquid hydrocarbon from the amine solution.
 Hydrocarbon buildup in the flash drum should be monitored and
hydrocarbons should be skimmed periodically via the facilities provided on
the flash drum.
7.1.2 Finely  Check the rate of flow through the amine filter; it should not exceed the
divided solids design rate. The flow rate through this filter also should not be significantly
less than the design rate.
 Replace and/or clean the amine filter media to provide adequate
particulate filtration.
 Make sure that the amine filter elements conform to the original
specifications.
 Monitor the differential pressure across this amine filter and change-
out the elements before the pressure drop reaches the critical maximum
(20 psi for SU-F-2002 and SU-F-2004; 30 psi for SU-F-2003). If the filter
pressure drop becomes stable, either the amine solvent is relatively clean
or the filter media is discharging the solid fines.
 Check the instrument taps for plugging, if the flow rate is erratic and/or
the absorber bottoms level is unstable (rapid movement up and down).
 The common source of particulates during startup is FeS.
Document No.:
149-RP-PR35-0003.01
MANUAL
7.1.4 Organic  Minimize the introduction or organic acids (hydrocyanic, formic, acetic,
acids naphthionic, and thiocyanic) by washing gas streams from coking and
cracking operations. These acids react with amine to form heat stable
salts (HSS).
7.1.5 Antifoam  Antifoam addition should be about 25 wppm per shot and should not
exceed 100 wppm /day. Excess antifoam has a tendency to stabilize the
foam.
 Do not mix different antifoams.
 Do not repeat anti-foam dosage for about 4-6 hours.
7.1.6 Field  Refinery materials groups should be consulted prior to adding any
corrosion inhibitors corrosion inhibitor to the amine solution.
7.1.7 Make-up  Use pure condensate for make-up.

water  Do not use raw water for make-up.
 Do not use boiler feed water (BFW) for make-up.
7.1.8 Valve  Replace all soap-based greases used in the unit valves with grease
grease that does not contain surfactants.
7.1.9 New  All new equipment or piping must be degreased prior to using in amine
equipment / piping service. This is typically done by washing the equipment/ piping with a
weak alkaline wash. Use either: 0.5 wt% DEA, or 0.3 wt% sodium
carbonate (Na2CO3) or 0.3 wt% sodium hydroxide (NaOH).
7.1.10 Phosphates  Wash the carbon bed with hot condensate until the phosphates are
from unwashed reduced.
activated carbon  Use vendor procedures for commissioning the Carbon bed.
Document No.:
149-RP-PR35-0003.01
MANUAL
7.2 AMINE SOLUTION DETERIORATION
7.2.1 Amine  Refer to Section 7.3.5, Amine Solution Color Change - Brownish
oxidation
7.2.2 Heat stable  Monitor for increase of solution viscosity and corrosivity, plus
salts decreased activity. Also regularly (monthly) test for amine heat stable salts
in the lean amine solution.
 Maintain the heat stable salt content below 10% of the titratable amine
concentration (e.g. a 25 wt% DEA should contain no more than 2.5% heat
stable salts)
 Online addition of NaOH, KOH, Na2CO3 or K2CO3 is not
recommended since the heat stable salts stay in the solution and may
potentially affect the H2S level in the treated gas. If any of the chemicals
are added to the amine system, then reclaiming will be required at a later
date to remove the Na+ or K+ ions.
 Amine activity is a function of the amine strength less the presence of
amine heat stable salts and/or amine degradation products.
7.2.3 Organic  Monitor loss of amine activity caused by organic acid neutralization of
acid formation the amine solution.
 Periodically measure the lean amine solution for the presence of
compounds resulting from organic acid contamination such as formates,
oxalates, acetates, glycolates, lactates, etc.
 Identify external source of organic acid introduction and reduce or
eliminate these materials.
7.2.4 Thermal  Eliminate hot spots (over 300F) in the amine system and high skin
decomposition temperatures in the reboiler potentially caused by superheated steam.
Make sure that only saturated steam is being supplied to the amine
regenerator reboiler.
Document No.:
149-RP-PR35-0003.01
MANUAL
7.2.5 Chemical  Monitor overall amine losses.

reaction  Check for presence of carbonyl sulfide (COS), hydrogen cyanide
(HCN), carbon monoxide (CO), mercaptans (other than H2S) and carbon
disulfide (CS2) in the inlet gas feed.
 Eliminate high temperature regeneration system production of amine
derivatives like piperazine, by using only saturated steam in the amine
regenerator reboiler.
7.2.6 Inorganic  Check the amine solution periodically for compounds caused by
acids inorganic acid contamination such as chlorides, sulfites, sulfates, thio-
sulfates, cyanates, thio-cyanates, nitrates, etc.
 Try to find the source of these compounds and prevent them from
forming and/or eliminate them from the amine system.
Document No.:
149-RP-PR35-0003.01
MANUAL
7.3 AMINE SOLUTION COLOR CHANGE

 None
7.3.1 Bright and  Blue or green or straw (pale yellow) tinge is okay as long as the
clear solution remains clear.
 Keep monitoring the color to avoid further deterioration of the amine
7.3.2 Grayish solution.
cast  It is okay if the solution is a pale, dull gray if the solution remains
transparent.
 Try to identify the source of the erosion and/or corrosion that is
7.3.3 probably generating iron sulfide particulates faster than they are being
Translucent black removed.
 Watch for erratic flow or signs that the bottoms level in the absorber
seems to be unstable, which may indicate that orifice taps on flow meters
and level taps are getting plugged.
 At this stage, usually objects can barely be seen through a sample;
and, after about ten minutes settling, there is a small amount of sediment
in the bottom of the sample.
 Take immediate steps to improve the amine filtering operations such
7.3.4 Opaque as replacement of the filter elements.
black  Prevent bypassing of the particulate filter.
 Change or clean the filter media daily or as often as required.
 Monitor the pressure drop across the particulate filter and the carbon
bed, if applicable.
 Maybe a corrosion inhibitor for the amine system is needed. But test
the corrosion inhibitor in the lab to ensure it does not cause the amine
solution to foam.
 Vent any noncondensibles from the reboiler steam chest.
 Check that regenerated amine is reaching the reboiler.
 Check that there is sufficient regenerator reflux flow.
 Take samples of lean amine and reboiler feed and confirm that both
have approximately the same acid gas concentration (H2S + CO2).
 Make sure the reboiler steam supply is saturated steam.
 Prevent flashing (to reduce corrosion) of the rich amine in the lean/ rich
exchangers by holding a back pressure on these exchangers with the
regenerator feed control valve.
Document No.:
149-RP-PR35-0003.01
MANUAL
7.3.5 Brownish  Take steps to prevent air from getting into the amine solution, which
(Ammonia Odor) can oxidize the amine forming a corrosive chemical.
 Blanket amine storage tanks, surge vessels and sumps with an inert
(non-oxygen) containing gas.
 Check to see if oxygen is coming into the amine absorber with the
feed gas.
 Perform preventative maintenance on the amine solutions pumps.
Check packing glands for leaks or other signs of failures.
Document No.:
149-RP-PR35-0003.01
MANUAL
7.4 AMINE LOADING / CONCENTRATION
7.4.1 Amine  Check amine strength regularly.

losing strength  Make sure that the amine strength determination in the lab can
distinguish between amine strength and heat stable salt concentration.
 Check lean amine and make-up water for total dissolved solids (TDS).
Higher TDS for amine sample indicates leaking amine water cooler if
there is one OSBL.
 Check inlet water pressure and outlet amine pressure for each cooler
if there is one OSBL.
 Block in CW inlet and outlet valves and open water vent or drain
valves on the exchanger. When exchanger is almost drained, check
drain with pH paper. A + 10 pH indicates a leaking exchanger.
 Check lean amine and make-up water for TDS. Lower TDS for lean
amine indicates steam or condensate is entering amine system.
 Check that condensate make-up block valve is closed.
 Block in cross connections between amine system and sour water
system (e.g., pump-outs, etc.)
 Check for regenerator reboiler tube leak by injecting a small quantity of
tracer chemical into the steam supply. Analyze regenerator bottoms
for tracer.
7.4.2 High  Rich amine loadings are a function of the absorber feed rates, H2S,
concentration / and CO2 content in the absorber feed streams, amine flow rate, amine
loading strength, and lean amine loadings. Verify that the amine flow rate and
absorber feed rates are close to the design ratio. Verify that the lean
amine acid gas loadings are at the design values (0.02 moles of total acid
gas per mole of amine or lower). Verify that the amine strength is at the
design value (25 wt% DEA). If any of these variables is off, adjustments in
the lean amine flow rate may be required to maintain proper rich amine
loadings
 Maintain recommended amine concentration, acid gas loading,
reboiler steam pressure and regenerator pressure to avoid increased
regeneration temperatures, difficulty in regeneration efficiency, and
potentially increased amine degradation products
Document No.:
149-RP-PR35-0003.01
MANUAL
7.5 FOULING
7.5.1 Iron  Refer to Finely Divided Solids in Section 7.1.2, "Foaming."

sulfide, iron oxide,  Refer to Brownish in Section 7.3.5, Amine Solution Color Change."
sand, pipeline  Review amine particulate filter operations. For more details also refer
dust, and mills to Finely Divided Solids in Section 7.1.2, "Foaming."
7.5.2 Calcium  Use only steam condensate for amine make-up water.
and magnesium  If steam condensate is not available, boiler feed water without the anti-
silicates, foulant chemicals usually added, is viable alternate amine make-up water.
carbonates,  Another alternate for amine make-up water is demineralized water.
sulfates
7.5.3 Sludge  Check amine filter operations.

 Do not exceed maximum allowable pressure differential across filters.
 The maximum allowable differential pressure across the main
particulate filter and the after filter downstream of the carbon bed is 25 Psi
each.
 The maximum allowable differential pressure across the carbon bed is
10 Psi.
 For more details also refer to Finely Divided Solids in Section 7.1.2,
"Foaming."
Document No.:
149-RP-PR35-0003.01
MANUAL
8 SHUTDOWN
When the Amine 2 Unit (SU) is to be shut down, the steps listed below should be followed:
 Step 8.1: Cease Rich Amine and Sour Hydrocarbon Gas flows
 Step 8.2: Clean-up Amine Inventory
 Step 8.3: Prepare for Maintenance and/or Amine Storage
Guidelines for these steps are described in the following sections. These activities are in
addition to standard plant safety and operating procedures for shutdown and startup
preparation. Details are provided primarily for the Regeneration Section. For further information
on upstream units, which affect the operation of Amine 2, please see the appropriate section
supervisor.
The shutdown operations should maximize removal of the acid gas (H2S and CO2) from the
circulating amine, especially for extended shutdowns, and provide for blanketing the process
equipment with inert gas (nitrogen) when the regeneration operation is terminated. This inert
gas blanket keeps air (oxygen) out of the Amine 2 system, which would cause degradation of
the amine solution.
There are no automatic emergency shutdown functions in the Amine 2 Unit. Any unit shutdown
will be manual.
8.1 CEASE AMINE AND SOUR HYDROCARBON GAS FLOWS
Purpose: The purpose of the following activities is to safely shut down Amine 2 when there
is no need to repair equipment.
General Guidelines:  Maintain amine flow through existing Amine Absorber (SU-
T-1)
 Strip the maximum amount of acid gas from the amine
solution.
Recommended Procedures:
The following stepwise procedures are recommended. These procedures are in addition to
standard plant safety and operating procedures for unit shutdowns.
Document No.:
149-RP-PR35-0003.01
MANUAL
8.1.1 Advise operators of off-site lean amine users (rich amine producers), operators of units
that are producers of sour gas feed to the Amine 2 Unit, and the SRU operators that Amine 2 is
going down.
8.1.2 Block flow of gas to the existing Amine 2 Absorber (SU-T-1). Maintain tower pressure
with suitable pressurizing gas (nitrogen or fuel gas) to permit circulation of amine solution from
the regenerator to the absorber and then to the Rich Amine Flash Drum for circulation back to
the regenerator. This ensures maximum removal of acid gas from the amine solution. (During
the 2013 FCC turnaround, a line will be added that allows circulation from the regenerator
directly to the Rich Amine Flash Drum.)
8.1.3 Block flow of feed streams to OSBL absorbers. If possible, maintain circulation of lean
amine until all rich amine has been replaced by lean amine. Transfer as much amine inventory
to Amine 2 as possible to minimize amine inventory in the OSBL absorbers. Be careful to avoid
introduction of hydrocarbons into the Amine 2 Unit.
8.1.4 Shutdown new Lean Amine Pumps (SU-P-2006 A-C). Block rich amine flow to OSBL
absorbers at the Battery Limits of the Amine 2 Unit. Block flow of lean amine to the Liquid
Ejector Drum (SU-D-2008). (During the 2013 FCC Turnaround, a line will be installed to allow
recycle from the new Lean Amine Pumps directly to the Rich Amine Flash Drum).
8.1.5 The Amine Acid Gas header should be blocked-in at the battery limits with acid gas
routed to the flare.
8.1.6 Shutdown the Liquid Ejector Pump (SU-P-2009 A or B) and bypass the regenerator
overhead vapor around the Liquid Ejector Compressor System.
8.1.7 Drain the contents of the ejector drum to the Rich Amine Flash Drum (SU-D-2007).
8.2 CLEAN-UP AMINE INVENTORY
Purpose: Remove remaining acid gases from amine.
General Guidelines:  Monitor lean and rich amine loading.

 Maintain normal operating levels, temperatures and pressures, if
possible.
Document No.:
149-RP-PR35-0003.01
MANUAL
8.2.1 Continue amine solvent recirculation through the Amine 2 Unit and continue stripping the
amine solvent until the regenerator feed has essentially the same CO2 and H2S composition as
the regenerator bottoms.
8.2.2 As the stripping proceeds and the amount of CO2 and H2S in the regenerator overhead
gas becomes depleted, feed nitrogen (or other oxygen free pressurizing gas) into the
regenerator to provide a slight positive flow of regenerator overhead gas to the flare. Nitrogen
should be fed into the regenerator by connecting a pressure regulated nitrogen hose to a
connection near the base of the tower or to the steam out connection.
Document No.:
149-RP-PR35-0003.01
MANUAL
8.3 PREPARE FOR MAINTENANCE AND/OR AMINE STORAGE
Purpose: Prepare amine for storage and equipment for maintenance as required.
General Guidelines:  Monitor system pressures.

 Monitor system temperatures.
8.3.1 When the stripping is complete, shut off the steam to the Regenerator Reboiler (SU-E-
2). The solvent may be cooled to at least 135°F by continued circulation through the Lean
Amine Coolers (SU-E-3 A/B until the 2013 FCC Turnaround and SU-E-2008 A/B after the 2013
turnaround). After the amine has been cooled to below 135°F, amine circulation can be
stopped.
8.3.2 The system should be blocked-in under a slight positive pressure of nitrogen. If a low
range pressure gauge is not already installed, one should be installed to measure the low
pressure.
8.3.3 Drain amine (as required for maintenance) to Amine Drain Sump (SU-D-4) and/or Amine
Storage Tank (SU-TK-1). Steam out the affected equipment and piping per the refinery standard
plant maintenance procedures.
8.3.4 When the unit cools, fuel gas and N2 pressures have to be reduced to atmospheric
pressure before the equipment can be opened for inspection and/or maintenance.
Document No.:
149-RP-PR35-0003.01
MANUAL
9 MAINTENANCE
With the exception of the Rich Amine Filters, SU-F-2002/2003/2004, there are no special
requirements for the maintenance of the Amine 2 Unit. The refinery should follow the regular
schedule maintenance requirement for the equipment/instruments to keep the unit running in
good conditions and also to meeting the lean amine loading requirement for the amine system.
Some of the items to be checked periodically include corrosion, cracking, etc. CB&I
recommends regular analytical testing of the rich and lean amine for H2S and CO2 loading,
amine strength and percentage of heat stable salt.
9 .1 Replacing the Cartridge in Rich Amine Prefilter, SU-F-2002

The normal pressure drop across the Rich Amine Prefilter (SU-F-2002), Rich Amine
Charcoal Filter (SU-F-2003), and Rich Amine Post Filter (SU-F-2004) is about 2 psi for
each unit. If the pressure drop as registered by the corresponding pressure differential
indicator is 10 psi or greater, the filter media should be replaced.
9.1.1 Rich Amine Filter Maintenace Procedure Summary

9.1.1.1 Bypass and block filter
9.1.1.2 Use lean amine to displace rich amine to process piping to Amine Regenerator
9.1.1.3 Use steam to displace lean amine to Rich Amine Flash Drum, SU-D-2007
9.1.1.4 Wash filter with condensate to Sour Water Disengaging Drum, GZ-D-2205
9.1.1.5 Steam out to Amine Sump, SU-D-4
9.1.1.6 Blind in filter using normal refinery procedures
9.1.1.7 Open filter and remove filter media (manufacturer does not recommend reuse)
9.1.1.8 Install new filter media and close filter
9.1.1.9 Displace air from filter with condensate (Condensate is used because drains and
vents can be used to ensure filling is complete.)
9.1.1.10 Put filter into service
9.1.2 Displacing of Rich Amine Using Lean Amine (SU-F-2002)

9.1.2.1 Open the 8” bypass valve around the filter.
9.1.2.2 Close the 8” inlet valve to the filter. The 8” outlet valve should remain open.
9.1.2.3 Swing the Figure 8 blind downstream of PCV-0146 in the lean amine line to the
open position following normal plant procedures.
9.1.2.4 Open the 2” gate valves upstream and downstream of PCV-0146.
9.1.2.5 Open the 1½” gate valve in the flushing line at the inlet to the filter. All valves in
the path between PCV-0146 and SU-F-2002 should now be open.
9.1.2.6 Slowly open the adjusting screw of PCV-0146 several turns. Let the lean amine
flow for several minutes until the pressure at PI-0145 stabilizes. Adjust PCV-
0146 until the pressure is 75 psig. Lean amine will now be flowing through the
Document No.:
149-RP-PR35-0003.01
MANUAL
filter, flushing the rich amine forward through its normal path. Allow the lean
amine to flow for approximately 15 minutes.
9.1.2.7 Close PCV-0146 by adjusting the set screw to the closed position.
9.1.2.8 Close the 2” gate valve upstream of PCV-0146.
9.1.2.9 Close the 2” gate valve downstream of PCV-0146.
9.1.2.10 Swing the Figure 8 blind downstream of PCV-0146 in the lean amine line to the
closed position following normal plant procedures.
9.1.2.11 Close the 8” outlet valve from the filter.
9.1.3 Displacing of Lean Amine to SU-D-2007 Using Medium Pressure Steam (SU-F-2002)
9.1.3.1 Open both 1” block valves in the drain line from the bottom of the filter. Make
sure the bleed valves between the blocks are closed and plugged.
9.1.3.2 Make sure the 2” block valves in the filter flush line to GZ-D-2205 and the drain
line to SU-D-4 are closed.
9.1.3.2 Open the 2” block valve in the drain line to allow flow to go into the rich amine
relief header to SU-D-2007.
9.1.3.3 Swing the Figure 8 blind downstream of PCV-0188 in the medium pressure
steam line to the open position following normal plant procedures.
9.1.3.4 Open the 2” gate valve upstream of PCV-0188 and the 2” gate valve downstream
of PCV-0188.
9.1.3.5 Slowly open the adjusting screw of PCV-0188 several turns. Let the steam flow
for several minutes until the pressure at PI-0187 stabilizes. Adjust PCV-0188
until the pressure is 60 psig. MP steam will now flow through the filter, pushing
the lean amine out through the filter drain line to SU-D-2007. Allow the steam to
flow until the temperature at the filter outlet reaches 130 °F as measured by TI-
0170, indicating that all of the liquid has been pushed out of the filter.
9.1.3.9 It is not necessary to close the Figure 8 blind since the steam will be used again
in a later procedure.
9.1.3.10 Close the 2” block valve opened in step 3 to block flow from going to SU-D-
2007 .
9.1.4 Flushing of Filter to GZ-D-2205 Using Condensate (SU-F-2002)

9.1.4.1 Make sure the 2” block valves in the filter drain line to SU-D-2007 and the drain
9.1.4.2 Open the 2” block valve in the filter flushing line to allow flow to go to GZ-D-2205.
Document No.:
149-RP-PR35-0003.01
MANUAL
9.1.4.3 Swing the Figure 8 blind downstream of PCV-0186 in the condensate line to the
open position following normal plant procedures.
of PCV-0186.
9.1.4.5 Slowly open the adjusting screw of PCV-0186 several turns. Let the condensate
flow for several minutes until the pressure at PI-0185 stabilizes. Adjust PCV-
0186 until the pressure reaches 60 psig or the valve is wide open. Condensate
will now flow through the filter, flushing any residual material to GZ-D-2205.
Allow the condensate to flow for approximately 15 minutes.
9.1.4.9 Swing the Figure 8 blind downstream of PCV-0186 in the condensate line to the
closed position following normal plant procedures.
9.1.4.10 Close the 2” block valve opened in step 2 to block flow from going to GZ-D-
2205.
9.1.5 Steaming of Filter to SU-D-4 Using Medium Pressure Steam (SU-F-2002)

9.1.5.1 Make sure the 2” block valves in the filter flush line to GZ-D-2205 and the drain
9.1.5.2 Open the 2” block valve in the drain line to allow flow to go to SU-D-4.
of PCV-0188.
9.1.5.4 Slowly open the adjusting screw of PCV-0188 until the pressure reaches 60 psig
or the valve is wide open. MP steam will now flow through the filter removing
volatile components. Steam and condensate will flow through the filter drain line
to SU-D-4. Allow the steam to flow until the temperature at the filter outlet
reaches 150 °F as measured by TI-0170, then maintain the flow for
approximately 15 minutes.
9.1.5.8 Swing the Figure 8 blind downstream of PCV-0188 in the medium pressure
steam line to the closed position following normal plant procedures.
9.1.5.9 Close the 2” block valve opened in step 3 to block flow from going to SU-D-4.
9.1.5.10 Close the 1½” gate valve in the flushing line at the inlet to the filter.
9.1.5.11 Close both 1” block valves in the drain line from the bottom of the filter.
Document No.:
149-RP-PR35-0003.01
MANUAL
9.1.6 Replacing the Filter Media

The filter is now ready to be vented, isolated (blinded), and opened in accordance with
typical refinery practices. Once the filter is open, the media can be extracted and
replaced. The manufacturer does not recommend cleaning and reuse of the cartridges.
Once the filter media is replaced, the filter can be closed and isolating blinds removed.
9.1.7 Displacing Air with Condensate

Condensate can now be used to displace the air by using PCV-0186 in a manner similar
to 9.1.4 above except that the filter is not line up to any other process equipment.
Condensate is used because vents and drains can be used to determine when all the air
has been removed. Once the filter is full of condensate, the condensate can be blocked
and the filter is ready to be placed in service.
If desired, the filter can be steam before filling with condensate. However, the filter must
be left open to the atmosphere or GZ-D-2205 during the subsequent filling with
condensate to avoid pulling a vacuum.
9.1.8 Placing Filter Back in Service

Once the filter is filled with condensate, all vents and drains closed, and condensate
blocked, it can be placed into service by slowly opening the outlet block valve and the
slowly opening the inlet block valve thus displacing the condensate to the Amine
Regenerator. Once the filter is on-line, the bypass can be closed.
9.2 Replacing the Filter Media for SU-F-2003 and SU-F-2004

Use similar procedures for replacing the filter media for SU-F-2003, Rich Amine
Charcoal Filter, and SU-F-2004, Rich Amine Post Filter. Because of its larger volume,
any liquid flushing of SU-F-2003 should be allowed to run for approximately 1 hour.
Opening the bypass for SU-F-2003 also bypasses SU-F-2004. This arrangement
ensures that the Charcoal Filter is not operated without the Post Filter, thus preventing
the introduction of solids into the circulating amine solution. However, the two filters can
be flushed and opened separately, especially if only the Post Filter requires a media
replacement. If both filters are to be opened, they can be flushed as a single unit.
Document No.:
149-RP-PR35-0003.01
MANUAL
APPENDICES
10.1 Appendix 1 - Analytical Tests
10.1.1 DEA in Lean Amine Solutions
10.1.1.1 Scope
This method describes a procedure for the determination of the “free” heat regenerable
diethanolamine (DEA) in lean amine solutions. The resulting titration includes the “free”
DEA, which is chemically bound to hydrogen sulfide, carbon dioxide, carbonyl sulfide,
and carbon disulfide. It does not include the DEA, which is chemically bound to strong
acids or to organic acids such as formic acid and acetic acid; nor does it include DEA that
has been converted to products such as amide and oxazolidone.
10.1.1.1 Method Summary
After adding excess 0.5N hydrochloric acid (HCl), the sample is titrated in aqueous
solution with 0.5N sodium hydroxide (NaOH) to either a visual brom cresol green or
potentiometric end point.
10.1.1.2 Apparatus
a. pH Meter and Titration Assembly  consists of a glass and calomel electrode with
an electrode holder, a magnetic stirrer and stirring bar, and 250 ml tall-form electrolytic
beakers.
b. Erlenmeyer Flasks  250 ml.
c. Burette, 25 ml  graduated in 0.05 ml increments.
10.1.1.3 Reagents
a. Hydrochloric Acid (HCl) 0.5N aqueous solution.

b. Sodium Hydroxide (NaOH) 0.5N aqueous solution.
c. Brom Cresol Green/Methyl Red Mixed Indicator.
10.1.1.4 Procedure
Weigh 1.0 to 1.5 grams of sample from a weight pipette into an Erlenmeyer flask
containing 40 ml of 0.5N HCl. Add 50 to 75 ml of water and 4 to 5 drops of brom cresol
green/methyl red mixed indicator. Shake well, then titrate excess HCl with 0.5N NaOH.
Document No.:
149-RP-PR35-0003.01
MANUAL
10.1.1.5 Calculation
(ml 0.5N HCl x N) – (ml 0.5N NaOH x N) x 11.916 = %DEA

Sample Weight
10.1.2 Foaming Tendency of Amine Solutions
10.1.2.1 Scope
An empirical method is described to determine the presence of surface active impurities

in amine solutions that lead to excessive foaming.
Note: There are a number of similar procedures for testing foaming, but all are
empirical. This method was developed as the simplest procedure that would indicate the
required information. Directions must be followed closely for reliable results. This
procedure follows closely the one published by Tretolite Division, Petrolite Corp., Bulletin
04-050, June 1964.
A sample of amine solution is brought to testing temperature. Nitrogen is bubbled

through the amine at a controlled rate. The volume of foam and the time required for
collapse of the foam after the gas flow stops is a measure of foaming tendency.
10.1.2.3 Apparatus
a. Graduated Cylinder 1000 cc; fitted with a two hole rubber stopper, one to fit
the glass inlet tube, and the other of any size sufficient to allow free passage of gas in
and out of the graduate.
b. Gas Diffuser Stone  One inch, attached to a 6-8 mm glass inlet tube with a short
length of Tygon tubing. (Gas diffuser stone is available from Fisher Scientific Company,
Catalog #11-139 or Central Scientific, Catalog #20970.)
c. Flowmeter  Calibrated at 600 cc/min of nitrogen.
d. Constant Temperature Baths suitable for immersing most of the 1000 cc

graduated cylinder and capable of maintaining a temperature of 80ºC (±1ºC).
e. Stop Watch or Timer.
Document No.:
149-RP-PR35-0003.01
MANUAL
10.1.2.4 Reagents
a. Sterox AJ (Monsanto Chemical Company)  For cleaning the dispersing stone.
b. Nitrogen  Plant nitrogen or in cylinders under pressure.
10.1.2.5 Equipment Operation Notes
a. Thoroughly clean the equipment for reliable results. After testing amine solutions,
wash the graduated cylinder with strong soap or detergent using a long handled brush.
Rinse the graduate several times with water, then with acetone, and air dry.
b. The gas dispersing stone is cleaned by flushing a solution of Sterox AJ through

the stone with the aid of a rubber squeeze bulb. The stone is then flushed well with
distilled water. After wiping the glass tubing with acetone on a tissue or clean rag, the
stone is dried by blowing air through it.
10.1.2.6 Procedure
a. Pour a 200 cc sample of amine solution into the 1000 cc graduate. Place the gas
dispersing stone in position as indicated in Figure 1.
b. Bring the sample to 80ºC in the constant temperature bath.
c. Bubble nitrogen through the solution at the rate of 600 cc/min.
d. Start the timer when bubbles first come out of the gas dispersing stone. After 60
seconds, record the volume reading in cc's at the top surface of the foam.
e. Stop the flow of gas and record the time for the foam to collapse.
Foam Volume = (Volume at Surface of Foam)  200; cc
10.1.3. Carbon Dioxide in Lean Amine Solution,

Gas Chromatographic Rapid Control Method
10.1.3.1 Scope
This method describes a rapid control procedure for determining carbon dioxide in lean
amine solution.
Document No.:
149-RP-PR35-0003.01
MANUAL
A sample of lean amine is injected by syringe into the heated injection port of a thermal
conductivity gas chromatograph. The carbon dioxide-amine complex is decomposed
thermally and the carbon dioxide is separated and emerges from a silica gel column.
The concentration is calculated by comparison with known samples.
101.3.3 Apparatus
a. Thermal conductivity gas chromatograph. An instrument which has an injection

port that can be heated to 250ºC is required. A Perkin-Elmer Model 154 has been used
for this purpose.
b. Micro-syringe, 1-10 microliters.
10.1.3.4 Column Preparation
The column is 3/16 inch x 15 feet and is packed with 50-60 mesh silica gel. The silica gel
should be dried at 150ºC in an oven for several hours before packing into the column.
10.1.3.5 Procedure
a. Adjust the instrument to the following conditions:

Injector Temperature: 250ºC
Column Temperature: 80ºC
Carrier Gas: Helium at 100 cc per minute
Sample Size: 1-5 microliters depending upon concentration
Since the lean amine is absorbed in the column, the column must be replaced
periodically and the injection port cleaned at the same time. Some instruments have
glass injection ports available as an accessory. The use of these glass sleeves, which
are discarded after injecting several samples, makes it easier to keep the injection port
clean.
b. To calibrate the instrument, prepare known solutions of carbon dioxide in fresh

amine by adding metered amounts of gaseous carbon dioxide to weighed quantities of
amine. Then inject samples into the chromatograph from one or more of these known
solutions. Calculate the area on the chromatogram.
Document No.:
149-RP-PR35-0003.01
MANUAL
Determine the concentration of carbon dioxide in the lean amine by the ratio of the CO2
peak areas of the known sample and the unknown sample.
10.1.4. Carbon Dioxide in Lean Amine Solutions,

Gasometric Method
10.1.4.1 Scope
This method describes a procedure for the determination of CO2 in lean amine. The
method described here is probably the simplest and the quickest for field use. However, it
is limited to CO2 in the lean amine.
A sample is taken at full system pressure in a stainless steel pressure vessel. A portion
of the sample is introduced into 25 wt.% sulfuric acid and the gas evolved is measured in
a gas burette. The volume of CO2 is corrected for temperature, pressure, and for the
volume of sample added.
10.1.4.3 Apparatus
a. Pressure Vessels  Stainless steel of 100-200 ml capacity and fitted with needle
valves and a 0-300 psig pressure gauge.
b. Syringe Needle  18 gage, 2 inches long, soldered to a 1/4 inch Swagelok cap
nut.
c. Filter Flask and Rubber Serum Stopper.
d. Gas Burettes  Graduated 100 ml and 1000 ml.
e. Levelling Bulbs  200 ml and 2000 ml.

f. Nitrogen Cylinder and Reducing Valve.
g. Magnetic Stirrer.
Document No.:
149-RP-PR35-0003.01
MANUAL
h. Thermometer  0-50ºC.
i. Platform Balance  Mettler K-9 or equivalent.
j. Syringe  50 cc.
10.1.4.4 Reagents
a. H2SO4, 25 wt.%  Add 250 grams of reagent H2SO4 to 750 grams of crushed ice.
b. Acid Brine Solution  160 grams Na2SO4 per liter, acidified with H2SO4.
c. Methyl Red, 0.1% in 60% alcohol.
10.1.4.5 Sampling
The sample is taken in a stainless steel sample vessel at the operating pressure. Attach
a sample line as short as possible to the bottom of the sample vessel. Open the lower
valve and control the flow by the upper valve. Purge the sample vessel by purging
several sample vessel volumes through it. Close first the top valve and then the bottom
valve. The sample vessel pressure will drop as the sample vessel cools. Take the
sample to the laboratory for analysis.
10.1.4.6 Procedure
a. Set up the equipment as shown in Figure 2. Connect the nitrogen cylinder with
regulator to the top valve of the sample vessel and adjust the regulator pressure to 200
psig. Connect the syringe needle to the lower valve and tighten in position.
b. Add 50 ml of 25% H2SO4, a stirring bar, and a few drops of methyl red to the filter
flask, close with the serum cap and weigh accurately to ± 0.01 grams on a platform
balance. Place the flask and contents on the magnetic stirrer and connect the flask to
the gas burette.
c. Pressure the sample vessel to 200 psig with nitrogen from the cylinder by
adjusting the top valve on the sample vessel. Leave the nitrogen cylinder connected
during the operation.
d. Slightly open the lower valve and allow a few drops of sample to flow through the
syringe needle.
e. When the amine leaves the syringe needle without excessive bubbling, connect
the sample vessel with the flask by plunging the syringe needle through the serum
stopper on the filter flask.
Document No.:
149-RP-PR35-0003.01
MANUAL
f. Start the stirrer, set the gas burette to zero via the levelling bulb, and allow the
sample from the vessel to flow drop-wise into the acid. The CO2 is evolved smoothly and
the levelling bulb may be lowered at intervals to maintain approximately atmospheric
pressure in the system. The addition of 30 grams of sample will require 10 to15 minutes.
g. When sufficient amine sample has been added, as measured by the volume of
CO2 collected in the burette, close the sample valve and allow the system to equilibrate
for 5 minutes. Adjust the levelling bulb to exactly match the level in the gas burette and
not the volume of gas.
h. Remove the filter flask and weigh it. This weight minus the weight obtained in
step (b) above is equal to the sample weight less the weight of the CO2 which has
evolved. Note the temperature in the vicinity of the gas burette.
Note: It may be more convenient to weigh the sample vessel before and after
amine addition to determine the sample weight. In this case, the observed weight
includes the weight of CO2.
Lean amine may be weighed in a 30 or 50 cc syringe. Lean amine will not evolve CO2 at
atmospheric pressure but it should be protected to avoid picking up additional CO2 from
the atmosphere.
A more primitive device to measure the gas evolved can be made from a large (500 or
1000 ml) burette. The top is closed with a tightly fitting one-hole rubber stopper. The
bottom is connected to a class T-tube with rubber tubing. At the start, the burette is full of
brine. The top of the burette is connected with the filter flask. The side arm of the glass
tee is at the same level as the brine in the burette; that is, the gas system is at
atmospheric pressure. As gas is evolved, the brine is displaced and collected. At the end
of the sample addition and equilibration period, the glass tee is moved down until the
side arm is at the level of brine inside the burette. The volume of brine collected is the
volume of CO2 evolved.
10.1.4.7 Calculations
a. Correct the observed volume by subtracting the volume of amine sample added.
Assume that the specific gravity of the amine is 1.00.
(S)
V1  V0
(d )
Document No.:
149-RP-PR35-0003.01
MANUAL
b. Correct V1 to standard conditions.
( V 1 ) ( 273.2 ) ( P )
VC 
( T ) ( 760 )
c. Calculate the weight of CO2.
( VC ) ( 44.01 )
 grams CO 2 evolved
( 22 ,400 )
d.
where:
V1 = CO2 gas volume, evolved, ml
V0 = Observed burette volume, ml
S = Sample weight less the weight of CO2 evolved, grams
d = Sample density, gm/ml
P = Barometric pressure, mm Hg
T = Observed temperature, ºK = ºC + 273.2
VC = Gas volume corrected to standard conditions, ml
10.1.5 Hydrogen Sulfide in Gases, Iodometric Method
10.1.5.1 Scope
This method describes a procedure for the determination of hydrogen sulfide in gases in
the range of 0.1 to 30 gms/m3. It is the widely used Tutweiller method with slight
modifications. The method does not distinguish between hydrogen sulfide and
mercaptans and is unsuitable for use when these constituents are to be determined
separately. Thus, in the presence of mercaptans, it yields the apparent hydrogen sulfide
content.
A known gas volume in a burette is titrated with iodine by successively admitting small
increments of standard iodine solution into the burette and shaking it until the color with
the starch indicator persists. A blank test is performed and the hydrogen sulfide content
of the gas is calculated from the volume of standard iodine solution used in titrating.
10.1.5.3 Apparatus
Document No.:
149-RP-PR35-0003.01
MANUAL
a. Tutweiller Burette, 100 ml capacity  The apparatus consists of a burette with a

two-way stopcock at the bottom connected by means of a rubber tube to a levelling
bottle, and a three-way stopcock at the top with one branch connecting to a 10 ml glass-
stoppered cylinder graduated in 0.1 ml divisions, as illustrated in Figure 3. The other
branch of the stopcock is the gas sample inlet. The burette itself has only two
graduations, one at the 100 ml mark and the other at 110 ml.
b. Tutweiller Burette, 500 ml capacity  For the determination of low concentrations,

a 500 ml burette is used which has two graduations  one at the 500 ml mark and one at
the 520 ml mark.
c. Levelling Bottle, 250 ml  For use with the 100 ml burette.
d. Levelling Bottle, 1000 ml  For use with the 500 ml burette.
10.1.5.4 Reagents
a. Iodine Solution, Standard 0.01N

Prepare as follows: Add 3 gm of c.p. potassium iodide to 4 ml of distilled water in a one
liter volumetric flask and dissolve. Weigh 1.269 gm of c.p. iodine into a tared glass-
stoppered weighing bottle. Transfer the iodine to the flask, rinse the weighing bottle with
3 to 5 ml of concentrated potassium iodide solution, and add the washings to the flask.
Swirl the flask gently until the iodine has dissolved, add water up to the one liter mark,
and mix thoroughly. Store the solution in a clean glass-stoppered brown bottle.
b. Iodine Solution, Standard 0.02N

Prepare according to the procedure above, but use 6 grams of potassium iodide and
2.538 grams of iodine.
c. Starch Indicator Solution

Pulverize 2 gm of soluble starch and 10 mg of mercuric iodide with sufficient water to
form a thin paste. Add the paste to one liter of boiling water and continue boiling for 3 to
4 minutes. Allow the solution to cool and store in a glass-stoppered bottle. Immediately
before use, titrate the starch solution with 0.01N iodine solution until a permanent faint
blue color persists. Make a fresh solution whenever mold appears or when a distinct
blue color is not obtained with the iodine solution.
Document No.:
149-RP-PR35-0003.01
MANUAL
10.1.5.5 Sampling
Choose the volume of the sample in agreement with the expected hydrogen sulfide
concentration as described in the table below.
Standard
Iodine Sample
Expected H2S Concentration Solution Volume
0.07 to 3 gms/m3 (46 to 1973 ppmv) 0.01N 500 ml

0.3 to 15 gms/m3 (197 to 9865 ppmv) 0.01N 100 ml
0.7 to 309 gms/m3 (460 to 203,226 ppmv) 0.02N
10.1.5.6 Procedure
a. Rinse the graduated cylinder (at the top of the burette) twice with iodine solution.
Fill the cylinder and the bore of the stopcock leading to the burette with the standard
iodine solution and record the reading.
b. Fill the levelling bottle with starch solution which has been tested according to
Section 4C above, and connect to the burette. Turn the stopcock at the top of the burette
to connect with the gas inlet tube and raise the levelling bottle until the burette and the
inlet tube are filled with starch solution. Close the stopcock at the bottom of the burette.
Note: If some iodine solution gets into the burette while filling the stopcock bore,
the starch solution, which is colored by the iodine, must be flushed out of the gas inlet
tube of the burette until no more coloration is observed.
c. Ensure that the opening of the gas sample tube is clear and attach it to the inlet
tube of the burette with plastic tubing. Open the stopcock at the bottom of the burette
and lower the levelling bottle, drawing in gas until the level of the starch solution just
passes the 100 ml mark on the burette. Close the stopcocks and disconnect the gas
sample tube. Open the lower stopcock and raise the starch solution to the 100 ml mark
by raising the levelling bottle. Close the stopcock. Open the top stopcock to the air for a
moment to bring the gas to atmospheric pressure. Open the lower stopcock and lower
the starch level to the 110 ml mark to place the gas under reduced pressure. Close the
lower stopcock and disconnect the levelling bottle from the burette.
d. Turn the top stopcock to admit small amounts of iodine solution into the burette
and shake well after each addition. Continue the additions until the starch solution
assumes a faint but permanent blue color of the same intensity as that of the solution in
the levelling bottle. Do not confuse the blue color with the opalescent milky appearance
Document No.:
149-RP-PR35-0003.01
MANUAL
due to the separation of free sulfur, nor with a red color that will disappear on shaking.
Record the reading on the iodine graduated cylinder and subtract from the previous
reading to find the amount of iodine used. When extreme accuracy is required, correct
for temperature and pressure.
e. Blank  Determine the amount of iodine solution required to give the starch
solution a blue color in the absence of hydrogen sulfide, in the following manner. Draw
starch solution into the burette to the 110 ml mark, close the lower stopcock and
carefully add iodine solution from the graduated cylinder until the starch solution shows a
permanent blue color. Shake the solution after each addition of iodine. About 0.2 to 0.3
ml of iodine solution will be required. Make this determination for each fresh bottle of
starch solution.
Calculate the hydrogen sulfide content by means of the following equation.
(A  B) (N) (11.84) (1,000,000)

Hydrogen Sulfide, ppmv 
(V)
where:
A = Volume of standard iodine solution used for titrating the gas sample,
milliliters
B = Volume of standard iodine solution used for the blank, milliliters
V = Volume of the gas sample, milliliters
N = Normality of standard iodine solution
11.84 = This factor is the number of milliliters of H2S gas at 760 mm Hg and 60F
that is equivalent to one milliequivalent of I2 solution.
10.1.6 Hydrogen Sulfide and Sulfur Dioxide in Gases,

Hydrogen Peroxide Method A
10.1.6.1 Scope
This method describes procedures for the determination of hydrogen sulfide and sulfur
dioxide in gases. The method used is determined by the hydrogen sulfide content in the
gases. Method A is intended for testing gases having a hydrogen sulfide content of 0.1%
v to 5% v (1000 ppm to 50,000 ppm). Method B, described in Section G following, is for
testing gases with a hydrogen sulfide content of 0.001% v to 0.1% v (10 ppm to 1000
ppm).
Document No.:
149-RP-PR35-0003.01
MANUAL
10.1.6.2 Method Summary - Method A Gases
(Containing 0.1%v to 5%v Hydrogen Sulfide)
A measured volume of gas is passed through an acidified solution of hydrogen peroxide

in which the sulfur dioxide is oxidized to sulfuric acid, with the hydrogen sulfide passing
through unaffected. Then the gas is passed through an alkaline hydrogen peroxide
solution which oxidizes the hydrogen sulfide to sulfuric acid. The two absorption liquids
are titrated acidimetrically with methyl red as an indicator. The sulfur dioxide and
hydrogen sulfide contents are calculated based on the residual gas volume.
10.1.6.3 Apparatus
a. Gas Meter, Wet Type  With a capacity of 3 liters per revolution, provided with a
thermometer.
b. Gas Wash Bottles  Two 200 ml wash bottles; one is provided with a double-
bored rubber stopper and the other is provided with a sintered glass dispersion thimble
of porosity G-1.
c. Gas Wash Bottles  Two 200 ml wash bottles for the purification of air.
d. Stainless Steel Sampling Line  Provided with an electric heating coil capable of
maintaining a temperature of approximately 150ºC and a regulating valve.
e. Vacuum Regulator  Tall 500 ml cylinder filled with water and closed with a
double-bored rubber stopper, one hole to take an adjustable dip-tube, the other to take a
T-piece.
10.1.6.4 Reagents
a. Methyl Red Indicator Solution, 0.1%  Dissolve 0.1 gram of methyl red in 60 ml of
denatured alcohol and dilute to 100 ml with distilled water. Filter if necessary.
b. Hydrogen Peroxide Solution, 6%  Prepare by diluting 200 ml of 30% hydrogen

peroxide (containing less than 0.001% of SO4) to one liter distilled water.
c. Sodium Hydroxide Solution, Standard 0.5N , Aqueous  To prepare, dissolve 25

grams of sodium hydroxide in 25 grams of distilled water, allow any precipitate to settle,
filter through a plug of glass wool, and dilute with CO2-free distilled water to one liter.
Standardize against potassium bi-iodate, using methyl red as an indicator. Store in a
Document No.:
149-RP-PR35-0003.01
MANUAL
bottle fitted with a guard tube containing approximately 4% sodium hydroxide solution to
prevent carbon dioxide from entering the bottle. Re-standardize the solution at frequent
intervals.
d. Hydrochloric Acid, Standard 0.5N To prepare, add 45 ml of concentrated

hydrochloric acid (Sp.Gr. 1.19) to one liter of distilled water. Standardize by titration of an
accurately weighed quantity of sodium carbonate in 125 ml of CO2-free distilled water,
using methyl red as an indicator.
10.1.6.5 Sampling
Connect the absorption equipment directly to the sampling point on the gas line. Do not
allow the sample to cool below its dew point before it reaches the first absorption vessel.
Do not use glass tubing in this part since glass lines may promote the formation of
elemental sulfur from hydrogen sulfide and sulfur dioxide. Use stainless steel tubing and
stainless steel couplings.
10.1.6.6 Procedure
a. If the expected H2S content is 0.1 to 2.0%, introduce the following into the first
absorber: 25 ml of 6% hydrogen peroxide solution by means of a 25 ml graduated
cylinder; 25 ml of distilled water by means of a 25 ml graduated cylinder; and 1.0 ml of
0.5N hydrochloric acid by means of a pipette. Introduce the following into the second
absorber: 25 ml of 6% hydrogen peroxide by means of a graduated cylinder; 25 ml of
0.5N sodium hydroxide solution by means of a pipette.
b. If the expected H2S content is 2.0 to 5.0%, introduce the following into the first
absorber: 25 ml of 6% hydrogen peroxide solution by means of a 25 ml graduated
cylinder; 25 ml of distilled water by means of a 25 ml graduated cylinder; and 1.0 ml of
0.5N hydrochloric acid by means of a pipette. Introduce the following into the second
absorber: 50 ml of 6% hydrogen peroxide by means of a graduated cylinder; 50 ml of
0.5N sodium hydroxide solution by means of a pipette.
c. Flush the heated sampling line with the gas sample and assemble the apparatus
as shown in Figure 4. Preferably make all connections glass-to-glass or glass-to-metal.
d. Take a reading of the gas meter and then pass the gas under test through the
apparatus at a maximum rate of 25 liters per hour, regulating the rate with the valve in
the sampling line. Read the temperature of the gas at the meter and record this
temperature together with the barometric pressure.
Document No.:
149-RP-PR35-0003.01
MANUAL
Note: If the pressure of the gas sample is insufficient to overcome the

resistance in the apparatus, draw the gas through the apparatus by means of a vacuum
regulator placed after the gas meter. Adjust to the desired vacuum prior to analysis by
inserting the dip tube of the vacuum regulator to the correct position. During the
absorption, allow a small stream of air to bubble continuously through the regulator.
Regulate the gas sample flow rate by means of the valve in the sample line.
e. Stop the gas flow as soon as the required volume has passed through (see table
below). Then read the gas meter and the temperature of the gas again. Disconnect the
sampling line from the first absorber.
Expected Hydrogen Sample

Sulfide Content, Volume
Volume Percent ppm v Liters
0.1 to 0.5 1,000 to 5,000 10

0.5 to 2.0 5,000 to 20,000 5
2.0 to 5.0 20,000 to 50,000 5
f. After sampling has been completed, pass 10 to 15 liters of air, purified by

passing it through 0.5N sodium hydroxide solution and followed by an empty wash
bottle, through the absorption train at a rate of 60 liters per hour. This stripping is
necessary to transfer all of the dissolved hydrogen sulfide from the first wash bottle to
the second.
g. Titrate the contents of the first absorber with 0.5N sodium hydroxide solution
using methyl red as an indicator until the color changes from pink to yellow.
h. Make a blank test by preparing a mixture of 25 ml of 6% hydrogen peroxide

solution, 25 ml of distilled water, and 1 ml of 0.5N hydrochloric acid. Titrate this mixture
with 0.5N sodium hydroxide solution with methyl red as an indicator.
i. Titrate the contents of the second absorber with 0.5N hydrochloric acid with
methyl red as an indicator.
j. Make a blank test by titrating a mixture of exactly the same volumes of hydrogen
peroxide solution and sodium hydroxide solution as used in the second absorber, using
methyl red as an indicator. Refer to Section F, 6, a and b above.
Document No.:
149-RP-PR35-0003.01
MANUAL
a. Calculate the volume of residual gas in liters of dry gas at 0ºC and 760 mm Hg by
means of the following equation.
(V) (273) (B  P  p)
Residual Gas, liters 
(273  t) (760)
where:
V = Volume of gas sample used, liters
t = Average temperature of gas sample at the meter, ºC
B = Barometric pressure, millimeters of mercury
P = Gas pressure at the gas meter, millimeters of mercury
p = Vapor pressure of water at temperature t, mm of mercury
Note: When the sample is under pressure and the gas pressure at the gas
meter during the test does not exceed 20 mm of water (1.47 mm Hg), the influence of
the gas pressure (P) can be neglected. (P is negative if vacuum is used.)
b. Calculate the sulfur dioxide content of the sample expressed in percentage of the
residual gas, by means of the following equation.
( A  B ) ( N 1 ) ( 2.12 )
Sulfur Dioxide , % v 
(V 1 )
where:
A = Volume of sodium hydroxide solution used for the titration of the first
absorber, milliliters
B = Volume of sodium hydroxide solution used for titration of the blank test,
milliliters
N1 = Normality of sodium hydroxide solution
V1 = Volume of residual gas at 0ºC and 760 mm Hg, liters
c. Calculate the hydrogen sulfide content of the sample expressed in percentage of

the residual gas, by means of the following equation.
( C  D ) ( N 2 ) ( 1.12 )
Hydrogen Sulfide, % v 
(V 1 )
Document No.:
149-RP-PR35-0003.01
MANUAL
where:
C = Volume of hydrochloric acid used for titration of the second absorber,

milliliters
D = Volume of hydrochloric acid used for the titration of the blank, milliliters
N2 = Normality of the hydrochloric acid
10.1.7 Hydrogen Sulfide and Sulfur Dioxide in Gases,

Hydrogen Peroxide Method B
10.1.7.1 Scope
This method describes the procedure for testing of hydrogen sulfide and sulfur dioxide in
gases when the hydrogen sulfide content is 0.011%v to 0.1%v (10 ppm to 1000 ppm).
10.1.7.2 Method Summary  Method B Gases
(Containing 0.001%v to 0.1% v Hydrogen Sulfide)
A measured volume of gas is first passed through an acidified solution of hydrogen

peroxide in which the sulfur dioxide is oxidized to sulfuric acid, with the hydrogen sulfide
passing through unaffected. Then the gas is passed through an alkaline solution of
hydrogen peroxide, which oxidizes the hydrogen sulfide to sulfuric acid. The sulfur
dioxide is determined by acidimetric titration of the first solution with methyl red as the
indicator. The hydrogen sulfide is determined by turbidimetric titration of the second
solution. The sulfur dioxide and hydrogen sulfide contents are both calculated on the
residual gas.
10.1.7.3 Apparatus
a. Apparatus as described in Section F-3 above.
b. Photoelectric turbidity instrument such as:
1) Photoelectric Absorptiometer, Unicam Model SP-600 or equivalent, with

special cells, one of 50 ml capacity (dimensions  20 x 40 x 70 mm), one of 80 ml
capacity (dimensions  30 x 40 x 70 mm). The cell cover should have two holes
and be equipped with a miniature stirring device.
c. Microburette, 10 ml
Document No.:
149-RP-PR35-0003.01
MANUAL
10.1.7.4 Reagents
a. Hydrochloric Acid, 38%
b. Reagents as prescribed in Section F-4 above.
c. Barium Chloride Solution, Standard 0.00312N  Prepared by dissolving 0.3809

gm of barium chloride dihydrate in 200 ml of distilled water and diluting to one liter with
acetone (or methanol if the Lange Model J colorimeter is used).
Note: One milliliter of solution is equivalent to 50 micrograms of sulfur.
d. Barium Chloride Solution, Standard 0.000624N  Prepare as under C above,

using 0.0762 gm barium chloride.
Note: One milliliter of solution is equivalent to 10 micrograms of sulfur.
e. Electrolyte Solution  Dissolve 20 gm of magnesium chloride in distilled water

and dilute to one liter. Adjust the pH to 8.0 to 8.2 with concentrated ammonia.
f. 10% Sodium Chloride Solution- Dissolve 100 gm of sodium chloride in distilled

water to make one liter of solution.
g. Acetone, reagent grade.
h. Methanol, reagent grade.
i. Potassium Sulfate Solution, Standard  Prepare this solution by dissolving

0.0543 gm of reagent grade potassium sulfate in 400 ml of distilled water. Dilute to 1 liter
with reagent grade acetone or methanol.
Note: One milliliter of solution equals 10 micrograms of sulfur.
10.1.7.5 Sampling
See Section F-5 above.
10.1.7.6 Procedure
a. Introduce the following into the first absorber: 25 ml of 6% hydrogen peroxide by

means of a 25 ml graduated cylinder; 25 ml of distilled water by means of a graduated
cylinder; 1.0 ml of 0.5N hydrochloric acid by means of a pipette. Using a 25 ml
Document No.:
149-RP-PR35-0003.01
MANUAL
graduated cylinder, introduce the following into the second absorber: 25 ml of 6%

hydrogen peroxide; 15 ml of distilled water; 10 ml of 0.5N sodium hydroxide solution.
b. Proceed according to Section F-6-c and F-6-d, above.
c. Stop the gas flow as soon as approximately 10 liters of gas have passed through.
Read the gas meter and the temperature of the gas again. Disconnect the sampling line
from the first absorber.
d. Proceed according to Section F-6-f, F-6-g and F-6-h above.
e. Acidify the contents of the second absorber by adding 38% hydrochloric acid.
Use pH paper to check the acidity.
f. Introduce into a 500 ml Erlenmeyer flask, which has been cleaned by boiling with
distilled water for at least 5 minutes, and a quantity of absorber liquid from step e above.
g. Add 1.0 ml of 10% sodium chloride solution, place a ground-joint chimney of

about 3” height on the flash and evaporate the contents to a volume of approximately 10
ml. heated above 392F (200ºC). Remove the chimney as soon as the first dry spots are
visible in the flask. Wash the inner wall of the chimney down into the flask, using a small
amount of distilled water, and continue evaporation. When bottom and wall of the flask
are dry, heat the flask at the same temperature for another 10 minutes or until the smell
of nitrogen oxide is not observed any more.
Note: Overheating of the residue may lead to low results.
With experience, the addition of sodium chloride solution can be omitted. If more than
500 micrograms of sulfur are presumed to be present, transfer the contents of the
second absorber to a 100 ml volumetric flask, and use a pipetted aliquot from this
solution for the sulfate determination.
h. Cool the flask to room temperature. Add 5 ml of the electrolyte solution via a
pipette and dissolve the residue completely.
i. The final steps in the sulfate content determination are carried out with the aid of
a photoelectric absorptiometer. The following procedures are for this sulfate
determination using the Unicam SP-600 Spectrophotometer or the Lange Model J
Colorimeter, respectively.
Document No.:
149-RP-PR35-0003.01
MANUAL
10.1.7.7. Unicam SP-600 Spectrophotometer
a. Carefully clean a 50 ml cell if it is expected that less than 100 micrograms of

sulfur are present, or an 80 ml cell for larger amounts. Transfer the contents of the
Erlenmeyer flask from step G-6-h above, quantitatively to this cell, using 15 ml of
acetone for the 50 ml cell or 55 ml for the 80 ml cell. With a pipette add 1.0 ml of the
potassium sulfate solution.
Note: The addition of potassium sulfate is intended to promote the

crystallization of barium sulfate, which may be retarded in case of very low sulfur
contents.
b. Clean the outer walls of the cell carefully, preferably by means of optical paper.
Place the cell in the instrument and start the stirrer. If the solution remains turbid,
probably due to precipitated sodium chloride, add 1 or 2 drops of distilled water. Set the
wavelength at 375 microns.
Note: Persistent turbidity at this stage indicates the presence of interfering ions.
c. Titrate, observing the following:
1) When it is expected that the amount of sulfur is less than 25 micrograms,

use 0.000624N standard barium chloride solution.
2) When it is expected that the amount of sulfur is more than 25

micrograms, use 0.00312N standard barium chloride solution.
3) When titrating, add at least 5 equal increments before the inflection point,
and then 4 increments in addition. Take a reading for each increment as soon as
a constant result is obtained. Plot the volumes of barium chloride solution against
the readings taken. The equivalence point is indicated by the point of intersection
of the two linear branches of the graph.
10.1.7.8 Lange Model J Colorimeter
a. Carefully clean the cell and transfer the contents of the Erlenmeyer flask from
step G-6-h above, quantitatively to the cell using 55 ml of methanol. Add 1.0 ml of the
potassium sulfate solution using a pipette.
Note: Any turbidity at this stage indicates the presence of interfering ions.
Document No.:
149-RP-PR35-0003.01
MANUAL
b. Clean the outer walls of the cell carefully, preferably by means of optical paper.
Place the cell in the right-hand compartment of the apparatus, bring the stirring device
with cell cover in position, and start the stirrer. Close the left-hand cell compartment,
insert the BG-12 filters, and adjust for highest sensitivity.
c. Titrate with 0.00312N standard barium chloride solution; add at least 5 equal
increments before the inflection point and 4 increments in addition. For each increment,
take a reading on the linear scale marked Abs as soon as a constant result is obtained.
Plot the volumes of barium chloride solution against the corresponding readings. The
equivalence point is indicated by the point of intersection of the two linear branches of
the graph.
Note: If the pointer of the galvanometer should overshoot the scale, readjust by
narrowing the diaphragm of the left-hand cell, not by adjusting the galvanometer
sensitivity.
10.1.7.9 First Blank Determination
Introduce into the cell 1.0 ml of 10% sodium chloride solution, 5 ml of the electrolyte
solution, 1 ml of the potassium sulfate solution (by means of a pipette), and the same
amount of solvent as used in the actual determination. Titrate according to Section G-7-c
and d, or Section G-8-c.
10.1.7.10 Calculations and Reporting
a. Calculate the amount of sulfur present in the sample by means of the following
equation:
Sulfur, micrograms = (Va - Vb)S
where:
Va = Volume of barium chloride solution used for the sample titration, milliliters
Vb = Volume of barium chloride solution used for the blank titration, milliliters
S = Sulfur equivalent of barium chloride solution, micrograms/milliliter
b. Calculate the sulfur content of the sample in ppm by weight using the following
equation:
( Va  Vb )S
Sulfur , ppm wt . 
W
Document No.:
149-RP-PR35-0003.01
MANUAL
where:
W = Weight of sample, grams
c. Report the sulfur content of the sample in ppm wt.
10.1.7.11 Repeatability
The following data should be used for judging the acceptability of the results obtained
(95% probability). Duplicate results by the same operator should not differ by more than
the following amounts:
Unicam SP-600 3 micrograms or 3%, whichever is larger

Lange Model J 8 micrograms or 8%, whichever is larger
Note: Make a second blank test using 25 ml of 6% hydrogen peroxide solution,

15 ml of distilled water, and 10 ml 0.5N sodium hydroxide solution, following the
procedure described starting at Section G-6. Do not add sodium chloride solution.
a. Calculate the sulfur dioxide content of the sample using the results from the
second blank test according to the equation in Section F-7 above.
b. Calculate the hydrogen sulfide content of the sample by means of the following
equation.
( E  F ) ( 0.699 )
Hydrogen Sulfide, ppmv 
(V 1 )
where:
E = Total quantity of sulfate sulfur as calculated in Section G-7-a, micrograms
F = Quantity of sulfate sulfur as determined in Section G-10-a, micrograms
V1 = Volume of residual gas at 0ºC and 760 mm Hg, liters
Note: The Method B described above in this Section G is from the Shell
procedure SMS-1770.
Document No.:
149-RP-PR35-0003.01
MANUAL
10.1.8 Hydrogen Sulfide, Mercaptans and Carbonyl Sulfide in Gases,

Electrometric Titration
10.1.8.1 Scope
This method describes procedures for determining hydrogen sulfide in concentrations as

low as 2 mg per cubic meter (1.3 ppmv), mercaptans in concentrations as low as 4 mg
per cubic meter (1.9 ppmv), and carbonyl sulfide in concentrations as low as 2 mg per
cubic meter (0.7 ppmv). Application of the method in the presence of hydrogen cyanide
may lead to erroneous results, however.
a. Hydrogen sulfide and mercaptans are removed from the gaseous sample by
passing it through a scrubber containing aqueous sodium hydroxide solution. The
carbonyl sulfide is removed by passing the gas through a second scrubber containing an
alcoholic solution of monoethanolamine. The separate solutions are then titrated
electrometrically with a silver nitrate solution, using as an indicator the electrical potential
between a glass or acetate reference electrode and a silver-silver sulfide indicating
electrode.
b. The end points for hydrogen sulfide and mercaptans (first absorber) are indicated
by separate inflections in the millivolts-milliliters curve, characteristic of the complete
precipitation of silver sulfide and silver mercaptide.
c. A substituted urea derivative is formed by the reaction between carbonyl sulfide

and monoethanolamine in the second absorber. During the titration two moles of silver
nitrate are consumed by each mole of carbonyl sulfide, the silver being precipitated as
black silver sulfide.
10.1.8.3 Apparatus
a. Absorption Train Consists of two 125 ml gas washing bottles with extra course
fitted cylinders. Wrap the second absorber with black tape, or provide other means of
light shielding.
Note: It is particularly important to use very coarse porosity gas dispersing

cylinders since carbonyl sulfide has been found to be retained by fine porosity
dispersers.
b. Flow Control Valve  A stainless steel 1/8” needle valve. For samples taken in
the liquid state, means of heating the valve must be supplied.
Document No.:
149-RP-PR35-0003.01
MANUAL
c. Gas Meter  Wet type, having a measuring capacity of about 3 liters per
revolution and a cumulative register up to about 300 liters. The meter should be
equipped with a thermometer and a water manometer for measuring the gas
temperature and pressure, respectively.
d. Tall-Form Beaker, 250 ml
e. Titration Burette
10.1.8.4 Reagents
Unless otherwise indicated, it is intended that all reagents conform to the specifications
established by the Committee on Analytical Reagents of the American Chemical Society,
where such specifications are available.
a. Ammonium Hydroxide, Concentrated (Sp.Gr. 0.90)
b. Monoethanolamine Solution, 5 wt.% in 99% isopropyl alcohol
c. Nitrogen, High Purity, Water Washed, Oxygen-Free A gas of suitable purity may
be obtained by passing ordinary cylinder nitrogen through a tube containing copper
gauze heated to 800oC.
d. Silver Nitrate Solution, Standard 0.1N Alcoholic  To prepare 1 liter of solution,

dissolve 16.99  0.01 grams of crystalline silver nitrate (which has been previously
pulverized, dried at 150oC for 1 hour, stored in a glass-stoppered bottle) in 150 ml of
distilled water, and diluted to 1 liter with refined 99% peroxide-free isopropyl alcohol.
Note: It is important to pass the isopropyl alcohol through a column of activated

alumina to remove peroxides that may have formed on storage. Failure to remove
peroxides will lead to low results and indistinct end points. Denatured (SD-3A) ethyl
alcohol can be substituted for isopropyl alcohol without being concerned about peroxide
formation.
e. Silver Nitrate Solution, 0.01N Alcoholic  Prepare daily by exact dilution of the
standard 0.1N silver nitrate solution with 92% peroxide-free isopropyl alcohol.
Note: Aqueous silver nitrate solutions may be used when it is known that only
hydrogen sulfide is present.
Document No.:
149-RP-PR35-0003.01
MANUAL
f. Sodium Hydroxide Solution, 30 wt.% Aqueous  To remove dissolved oxygen,

purge the solution with a stream of nitrogen for 10 to 15 minutes each day prior to use.
g. Titration Solvent, Acidic  To prepare 1 liter of solution, dissolve 2.7 gm. of

sodium acetate trihydrate or 1.6 gm. of anhydrous sodium acetate in 20 ml of oxygen-
free water, pour into 975 ml of peroxide-free 99% isopropyl alcohol (see Note above in
section 4-d), and add 4.6 ml of glacial acetic acid. To remove dissolved oxygen, purge
the solution in a flame and spark-free area with a stream of nitrogen for 10 to 15 minutes
each day prior to use. Keep the solution protected from atmospheric oxygen.
10.1.8.5 Sample
a. Samples for analysis may be taken directly from the line by making a connection
to the needle control valve of the apparatus through a stainless steel tube which is
resistant to corrosion and non-absorbent to sulfur compounds. Analyses should not be
made on samples taken in containers that are not corrosion resistant, or on samples
taken by water displacement.
b. The quantity of sample required for an analysis depends upon the hydrogen
sulfide and/or mercaptan content, and should be chosen so that a titration of 2 to 10 ml
of 0.01N silver nitrate solution will be obtained on each absorber solution. Normally, a
gas sample volume of 8 to 12 liters is adequate. Samples smaller than 3 liters should not
be used because of limitations in the accuracy of the gas meter.
c. If the expected carbonyl sulfide content is not the same magnitude as either the
expected mercaptan or the hydrogen sulfide content, it may be necessary to analyze two
portions of the gas sample. For example, if the H2S content is much higher than the COS
content, feed sample gas of sufficient volume to require 2 to 10 ml of 0.01N silver nitrate
solution when analyzing the first absorber solution for H2S. Leave the solution in the
second absorber. Then refill the first absorber with solution. Feed additional sample gas
of sufficient volume to require 2 to 10 ml of 0.01N silver nitrate solution when analyzing
the second absorber solution for COS. It is not necessary to analyze the first absorber
solution as the H2 content was determined after the first sample was taken. Pass the gas
sample through both absorbers in either case.
10.1.8.6 Procedure
a. Absorption
1) Assemble the gas absorbers in series as shown in Figure 5 and connect

the outlet tube of the second (shielded) absorber to the gas meter. Connect the
inlet tube of the first absorber to the flow control valve on the sample line and to
Document No.:
149-RP-PR35-0003.01
MANUAL
the rate control valve on the nitrogen gas line in such a way that either the
sample or the nitrogen may be passed through the absorbers without
disconnecting the apparatus from the system. Make all connections as short as
possible with glass tubing, joined either by short lengths of plastic (Tygon) tubing
or by ground-glass joints.
2) Place 20 ml of 30 wt.% aqueous sodium hydroxide solution in the first

absorber and 20 ml of 5 wt.% alcoholic monoethanolamine solution in the second
(shielded) absorber. Flush the assembled apparatus with about 25 liters of
nitrogen to displace all the air from the system. (The gas meter is used to
measure the volume of nitrogen.)
Note: Because mercaptans and sulfides are easily oxidized in an alkaline

solution, care must be taken to eliminate all dissolved oxygen in the caustic scrubber
prior to and following absorption of the mercaptans.
3) Record the initial gas meter reading and the temperature of the gas at the
meter. Pass the gaseous sample through the absorbers at a rate of 130 to 180
ml/min. until the required quantity (8 to 12 liters) of sample has passed through.
During this period, do not allow the pressure in the meter to exceed 20 mm of
water.
4) Stop the gas flow and record the meter reading, the temperature of the
gas at the meter, and the barometric pressure. Flush the assembly with at least
10 liters of nitrogen (see Note below) and disconnect the absorbers.
Note: It is important to remove all of the carbonyl sulfide from the caustic
solution with the nitrogen purge and transfer it to the second absorber containing the
monoethanolamine solution.
b. Titration
1) Hydrogen Sulfide and Mercaptan  Transfer all of the aqueous alkaline

solution from the first absorber to a 250 ml tall-form beaker. Dilute to 125 ml with
de-aerated distilled water, add 0.5 ml of concentrated ammonium hydroxide, and
titrate for sulfide and mercaptan using 0.01N silver nitrate solution according to
the procedure described in Section I of this appendix (following). If the total
titration to the second end point is less than 2 ml, repeat the analysis using a
larger sample. If the titration is greater than 10 ml, repeat the analysis using
either a smaller sample or an aliquot of the absorber liquid.
Document No.:
149-RP-PR35-0003.01
MANUAL
2) Carbonyl Sulfide  Transfer all of the alcoholic monoethanolamine

solution from the second absorber into a 250 ml tall-form beaker. Immediately
dilute to 125 ml with acidic titration solvent as prepared in Section H-4-g above.
Titrate the resulting solution using 0.01N alcoholic silver nitrate solution. If the
total titration falls appreciably outside the 2 to 10 ml range, repeat the analysis
using a larger or smaller sample or using an aliquot portion of the absorber liquid.
Note: The equilibrium between the carbonyl sulfide-monoethanolamine reaction

product and the silver nitrate solution is established slowly. During the titration, the
electrical potential increases greatly upon each addition of silver nitrate, afterwards
dropping to almost the original value. The titration time can be considerably reduced if,
instead of awaiting the return to the electrical potential to its original value, the next
addition be made as soon as it is observed that the electrical potential will drop. At the
end point, the electrical potential change is very great and no falling-off occurs.
a. Calculate the volume of gaseous sample taken, in liters of dry gas at standard
temperature and pressure, by means of the following equation.
Gas Volume, liters =
( VO ) ( 273 ) ( P  p )
Gas Volume , liters 
( 273  t ) ( 760 )
where:
VO = Observed volume of gas, liters
P = Barometric pressure, millimeters of mercury
t = Temperature of the gas, ºC, at the meter
p = Vapor pressure of water (mm Hg) at temperature t as given in the table

below
Temp. ºC mm Hg Temp. ºC mm Hg
16 13.6 28 28.3
18 15.5 30 31.8
20 17.5 32 35.7
22 19.8 34 39.9
24 22.4 36 44.6
26 25.2 38 49.7
Document No.:
149-RP-PR35-0003.01
MANUAL
b. Calculate the hydrogen sulfide, mercaptan and carbonyl sulfide as sulfur and
express in one of several units by means of one of the following equations.
( A) ( N ) ( K )
H 2 S as Sulfur 
(S)
( B  A ) ( N ) ( 2K )
RSH as Sulfur 
(S)
(C ) ( N ) ( K )
COS as Sulfur 
(S)
where:
A = Volume of standard silver nitrate solution, milliliters, used in titrating the

first absorber solution to the hydrogen sulfide end point.
B = Volume of standard silver nitrate solution, milliliters, used in titrating the
first absorber solution to the mercaptan end point.
C = Volume of standard silver nitrate solution, milliliters, used in titrating the
second absorber solution to the carbonyl sulfide end point.
N = Normality of the standard silver nitrate solution
K = Multiplier, as given in the table below, dependent upon the required
reporting units.
S = Amount of sample in units corresponding to reporting units in the table
below.
Reporting UnitsK S
mg. S/cubic meter 16,033 Vol, liters dry gas at STP

grains S/100 cu. ft. 699.2 Vol, liters dry gas at STP
wt. % as S 1.603 Weight, grams
ppm as S 11,207 Vol, liters dry gas at STP
To calculate the results in weight percent sulfur when the sample is measured by gas
volume, divide the results in milligrams per cubic meter by the vapor density of the
sample (grams per milliliter at 0ºC and 760 mm Hg pressure) and divide the quotient by
10,000,000. If the sample composition or molecular weight is known, the vapor density
may be calculated assuming ideal gases.
Document No.:
149-RP-PR35-0003.01
MANUAL
10.1.9 Sulfide and Mercaptans in Aqueous Solutions,

Electrometric Titration
10.1.9.1. Scope
This method describes procedures for the determination of sulfides and mercaptans,
either alone or in the presence of each other, in aqueous solutions. The procedure is
also applicable to the determination of sulfides and mercaptans in a refinery effluent
stream, provided the sample solutions are stabilized when collected. Any ion or radical
(e.g., bromide, iodine, or cyanide) that, in alkaline solution, precipitates a silver salt less
soluble than silver mercaptide, will interfere with the test. Substances capable of
reducing the silver ion to metallic silver in an alkaline solution also interfere. Dissolved
oxygen causes low results. Suspended material (such as elemental sulfur), which does
not react with silver ion, does not interfere and need not be removed.
The solution is titrated electrometrically with silver nitrate solution using as an indicator
the potential between a glass reference electrode and a silver-silver sulfide indicating
electrode. Under these conditions, the hydrogen sulfide is precipitated as silver sulfide,
and the mercaptan is precipitated as silver mercaptide. The titration curve has two
distinct inflection (end) points, one at the complete precipitation of silver sulfide and the
other at the complete precipitation of silver mercaptide. In the presence of hydrogen
sulfide, the method is applicable to C4 and lighter mercaptans, regardless of the
concentrations of mercaptans and hydrogen sulfide.
The basic purpose of the silver electrode is to measure the sulfide ion concentration in
the sample solution. The electrode is coated electrolytically with silver sulfide. For all
practical purposes, the measurement of sulfide ions is essentially an oxidation-reduction
potential measurement, where the concentration of the reduced form (the metal) is
constant. When immersed in the sample solution, the electrode reacts with the solution
and releases silver ions (Ag+). The concentration of silver ions that goes into solution is
dependent on the concentration of sulfide ions in the solution. The electrical potential
developed between the silver and its ions is related to the sulfide ion concentration.
10.1.9.3 Apparatus
Titration equipment consisting of a cell system containing a glass reference electrode

and a silver-silver sulfide indicating electrode (Figure 6), an electronic voltmeter with
integral titration stand and a 10 ml burette is required. The electrical potentials (millivolts)
described in this procedure are those normally obtained with Beckman glass electrodes
of present manufacture. Other makes of glass electrode may give somewhat different
Document No.:
149-RP-PR35-0003.01
MANUAL
electrical potentials, and in such cases the values given in the procedure are intended
for general guidance only. The algebraic signs of the meter readings are those realized
with the Shell-Precision Dual AC Titrometer. Other instruments generally use opposite
signs.
10.1.9.4 Reagents
Unless otherwise indicated, it is intended that all reagents conform to the specifications
established by the Committee on Analytical Reagents of the American Chemical Society
where such specifications are available.
a. Hydrochloric Acid, 20 wt.%  Prepare by mixing equal volumes of concentrated

hydrochloric acid (Sp.Gr. 1.19) and distilled water.
b. Silver Nitrate Solutions, Standard 0.1N and 0.01N , Aqueous.
Note: If desired, alcoholic silver nitrate solutions may be used. (Refer to Section
H-4 of this Appendix.)
c. Sulfide Stabilizer Solution  Prepare a suspension by dissolving 22 grams of zinc

acetate dehydrate and 40 grams of anhydrous sodium carbonate each in 200 ml of
distilled water and then mix (5 ml of this stabilizer will suffice for nearly 60 mg of sulfide
sulfur).
10.1.9.5 Sample
a. Because of the danger of partial loss of the sample by oxidation or evaporation, it

is recommended that samples be analyzed within an hour after they are taken. If this is
not practical, store the sample on ice (0ºC). In all cases, use completely filled, well-
stoppered, amber colored bottles.
b. Collect samples and stabilize within 3 minutes after collection, using 1 ml of zinc
acetate stabilizer solution for each 12 mg sulfide sulfur expected. At design conditions,
the lean amine solution is expected to contain about 0.003 wt.% H2S. This concentration
is equivalent to 2.8 mg S/100 grams of lean amine solution. Therefore, add about 0.3 ml
of stabilizer solution per 100 grams of sample.
c. The recommended combinations of liquid sample volumes and normality of titrant
are given in the table below. It is advisable to choose a sample of such size that no more
than 10 ml of 0.1N silver nitrate solution is required for the titration, as difficulties may
arise from the accumulation of large quantities of precipitate.
Document No.:
149-RP-PR35-0003.01
MANUAL
Expected Value of
[(0.5) (H2S) + RSH] Volume of Normality of
Wt.% as S Sample, ml AgNO2 Solution
Below 0.008 50 0.01

0.005 to 0.016 25 0.01
0.012 to 0.040 10 0.01
0.024 to 0.080 50 0.1
0.050 to 0.160 25 0.1
0.120 to 0.200 10 0.1
Above 0.200 5 0.1
10.1.9.6 Sample Preparation
Acidify the stabilized sample with 20 wt.% hydrochloric acid solution in a closed nitrogen-
scrubbed system. Flush with nitrogen to carry the hydrogen sulfide into the basic titration
solvent. Titrate the sample as described below.
10.1.9.7 Procedure
a. Accurately measure the required quantity of sample (see table in 5-c, above) into
a 250 ml tall-form beaker.
b. Place the beaker on the titration stand and adjust its position so that the
electrodes are about half immersed (see Figure 6). Fill the 10 ml burette with the silver
nitrate solution of the correct normality and place the burette in position in the titration
assembly so that the tip extends approximately 25 mm below the surface of the liquid in
the beaker.
Adjust the speed of the stirrer to give vigorous stirring without spattering. Record the
initial burette and meter (cell potential) readings.
c. Add suitable small portions of silver nitrate solution and, after waiting until a
constant potential has been established, record the burette and meter readings. During
some parts of the titration, especially when using 0.01N silver nitrate solution, 5 to 10
minutes may elapse before an unchanging potential is attained. Consider the potential
constant if it changes less than 6 mV/minute.
Note: If black silver sulfide is precipitated, tap the silver electrode to dislodge
the clinging precipitate and be sure that equilibrium has been reached before each
reading. If the potential (mV) readings obtained with freshly prepared electrodes are
Document No.:
149-RP-PR35-0003.01
MANUAL
erratic, it is possible that the electrodes are not properly conditioned. This difficulty
usually disappears in succeeding titrations, however.
d. At the start of the titration, and in regions between inflection (end) points, when
the electrical potential change is small for each increment of silver nitrate solution used,
add silver nitrate solution volumes as large as 0.5 ml. When the rate of change of
potential becomes greater than 5 mV per 0.1 ml, use 0.05 ml increments of 0.01N silver
nitrate solution.
Note: Although it is important to wait for equilibrium conditions, it is also

important that the titration time be as short as possible to avoid oxidation of the sulfur
compounds by atmospheric oxygen. Once started, a titration must never be interrupted
and resumed later.
e. Continue the titration until the rate of change of the cell potential is less than 2
mV per 0.1 ml of silver nitrate solution and the meter reading is approximately +200 mV.
Remove the titrated solution, rinse the electrodes well with water, wipe with a dry cloth,
and burnish the silver electrode lightly with a fine emery cloth.
10.1.9.8 Curve Interpretation
a. Plot the cumulative milliliters of silver nitrate solution added against the
corresponding cell potentials in millivolts. In the presence of mercaptans alone, the
initial cell potential should be between -50 and -350 mV. If sulfide is present, the initial
potential should be approximately -400 to -600 mV.
b. Select the end points at the most positive value of the steepest portion of each
break in the titration curve as illustrated by Figure 7. When either mercaptan or sulfide
only are present, the end point should occur in the neighborhood of +200 mV. When
present together, the sulfide end point will occur at about 400 mV.
a. Calculate the sulfide and mercaptide content as weight percent sulfur by means
of the following equations.
( A ) ( N ) ( 1.603 )
Sulfide, Wt .% as S 
( D ) (V )
( B  A ) ( N ) ( 3.206 )
Mercaptide, Wt .% as S 
( D ) (V )
Document No.:
149-RP-PR35-0003.01
MANUAL
where:
A = Volume of standard silver nitrate solution, milliliters, used in titrating to the
sulfide end point
B = Total volume of standard silver nitrate solution, milliliters, used in titrating
to the mercaptide end point
D = Density of sample, grams per milliliter
N = Normality of the standard silver nitrate solution
V = Volume of sample used, milliliters
b. To obtain the results in ppm (weight) as sulfur, multiply the values obtained
above by 10,000.
Document No.:
149-RP-PR35-0003.01
MANUAL
FIGURE 1
Apparatus for Foaming Test
Document No.:
149-RP-PR35-0003.01
MANUAL
FIGURE 2
Apparatus for Gasometric CO2 Determination
25 wt% H2SO4
Document No.:
149-RP-PR35-0003.01
MANUAL
FIGURE 3
Tutweiller Burette
Document No.:
149-RP-PR35-0003.01
MANUAL
Figure 4
Apparatus Assembly
Document No.:
149-RP-PR35-0003.01
MANUAL
Figure 5
Apparatus Assembly
Document No.:
149-RP-PR35-0003.01
MANUAL
FIGURE 6
Cell Assembly
Document No.:
149-RP-PR35-0003.01
MANUAL
FIGURE 7
Illustrative Titration Curves
Document No.:
149-RP-PR35-0003.01
MANUAL
10.2 Appendix 2 – Chemical Properties & Hazards (MSDS)
10.2.1 Hydrogen Sulfide
10.2.1.1 Properties
Formula H2S
Color Colorless
Odor Offensive odor characteristic of many mineral spring

waters; commonly referred to as odor of rotten eggs.
Corrosive Corrosive to eye and respiratory tissues. Attacks many

metals, forming sulfides.
Affinity for Water Water at room temperature absorbs approximately three

times its volume of hydrogen sulfide.
Specific Gravity 1.189 with respect to air.
Molecular Weight 34.08
Explosive Limits 4.3 to 46 percent by volume in air at room temperature.

The lower explosive limit at 130ºC (266F) is 3.7% by
volume.
Auto Ignition Temp. 260ºC (500F )
10.2.1.2 Hazards and Their Control
a. Physiological Effects
Hydrogen sulfide, even at low concentrations, acts as an irritant to the eyes and
respiratory tract. Low concentrations are easily recognizable by smell when first
encountered. However, the sense of smell is very unreliable for detecting hydrogen
sulfide and reliance upon it can, under certain conditions, prove very dangerous. High
concentrations, which have a sweetish odor, have a paralyzing effect on the olfactory
nerves and if inhaled may cause death. Even low concentrations, after prolonged
exposure, will fatigue the sense of smell to a point where the exposed person may fail to
detect the presence of the gas. The maximum allowable concentration is generally
Document No.:
149-RP-PR35-0003.01
MANUAL
recognized at 10 ppm by volume in air for an eight-hour regular working period. For a
period of up to 15 minutes, the maximum allowable concentration is 20 ppm by volume.
b. Fire and Explosion Hazard
Hydrogen sulfide is a flammable gas. It burns in air to form Sulfur dioxide and water with
the liberation of heat. Its explosive limits are 4.3 to 46 percent by volume in air at room
temperature.
c. Personal Protective Equipment
Since hydrogen sulfide is so rapidly fatal, supplied air or oxygen respirator equipment
with full-face mask should be used by all persons entering a contaminated area.
10.2.1.2 First Aid and Medical Treatment
Remove patient to fresh air or to a well ventilated room. If oxygen inhalation apparatus is
available and someone familiar with its use is present, oxygen should be given to
patient. Attempts to give oxygen by one not familiar with the use of the apparatus may
result in loss of valuable time or harm to the patient. If respiration has stopped, start
artificial respiration at once. Keep patient quiet and comfortably warm, but not hot. Call a
physician immediately. Do not give anything by mouth to an unconscious patient.
Eye irritation caused by exposure to hydrogen sulfide often becomes very painful and
requires special treatment by a physician, preferably an eye specialist. Keep patient in a
darkened room; apply an iced compress to the eyes; put ice cap on forehead; send for a
physician.
10.2.2 Sulfur Dioxide
10.2.2.1 Properties
Formula SO2
Color Colorless
Odor Pungent Odor
Corrosive Corrosive to eye and respiratory tissues. Attacks many
metals.
Specific gravity 2.264 with respect to air.
Document No.:
149-RP-PR35-0003.01
MANUAL
Sulfur dioxide even in low concentrations acts as an irritant to the eyes and respiratory
tract. Low concentrations are easily noticed by smell when encountered. High
concentrations, if inhaled, may cause death. For an eight hour work period, the industrial
hygiene standard is a maximum of 2 ppm.
b. Fire and Explosion Hazards
Sulfur dioxide reacts slowly with oxygen to form sulfur trioxide, the anhydride of sulfuric
acid. Because of the slowness of uncatalyzed oxidation, sulfur dioxide is not considered
to be flammable or an explosion hazard.
Since sulfur dioxide can be fatal, supplied air or oxygen respiratory equipment of
appropriate design with full-face mask should be used by all persons entering a
contaminated area.
10.2.2.3. First Aid and Medical Treatment
available and someone familiar with its use is present, oxygen should be given to the
Eye irritation caused by exposure to sulfur dioxide often becomes very painful and
requires special treatment by a physician, preferably an eye specialist.
10.2.3 Sulfur
10.2.3.1 Properties
Formula S, S2, S4, S6, S8
Molecular Weight 32.06, 64.12, 128.24, 192.36, 256.48
Vapor Specific Gravity 1.109, 2.219, 4.437, 6.656, 8.875
(all with respect to air)
Document No.:
149-RP-PR35-0003.01
MANUAL
Liquid Specific Gravity 1.803 with respect to water.
Liquid Viscosity Varies radically with temperature, decreasing from

approximately 12 cP at 118ºC (244F) down to
approximately 6.5 cP at 152ºC (306F), then
increasing back to about 12 cP at 160ºC (320F),
increasing very rapidly to over 10,000 cP at 163ºC
(326F).
Melting Point 119ºC (246F)
Flash Point 188ºC (370F) to 207ºC (405F) (range reported by

different sources)
Boiling Point 447ºC (837F)
Vapor Pressure 1 mm Hg at 183.8ºC (363F)
Auto Ignition Temperature 232ºC (450F)
Color Light yellow
Although sulfur dust is a nuisance, it is a very low toxic hazard, and only a moderate
explosion hazard when the dust is exposed to a flame. The principal danger lies in the
combustion of Sulfur to form SO2. Under these circumstances, the earlier paragraphs on
sulfur dioxide apply.
Prolonged or excessive exposure to sulfur dust and/or fumes can cause irritation of the
eyes, lungs, and breathing passages. It is recommended that anyone exposed to either
sulfur dust or fumes for continuous periods in excess of 30 minutes be equipped with
dust mask and goggles. Medical attention is usually not required for treating irritations of
this origin. However, if symptoms persist a physician should be consulted.
Because of the variations in the viscosity of liquid sulfur, it is very important to keep the
temperature of any liquid sulfur above 121ºC (250F) and below 160ºC (320F), not only
to prevent overloading of the sulfur pump, but to assure proper draining of any liquid
from the equipment to the sulfur storage pit.
Document No.:
149-RP-PR35-0003.01
MANUAL
After initial operation, a sulfur recovery plant may contain trapped sulfur in some
locations, which will burn at temperatures as low as 204ºC (400F) if excess air is
present. Permanent damage to plant equipment by overheating could result. Therefore,
during start-up and shutdown periods, all temperatures should be monitored, particularly
the reactor outlet temperatures. If a temperature begins to rise rapidly, the unit should be
shut down and cooled off with an inert gas purge.
Caution: Never operate the Air Blower for cooling so that it discharges into a hot
plant because possible sulfur fires in the equipment may result.
Some dissolved gases (including H2S and SO2) are present in the SRU molten sulfur
and evolves over a period of time and/or upon agitation.
10.2.4 Carbon Disulfide
10.2.4.1 Description
At ordinary room temperature and atmospheric pressure, carbon disulfide is a clear,

colorless liquid and is nearly odorless. It is also known by the name carbon bisulfide.
In the Sulfur Recovery Unit, it is not found in the liquid state, but in the gaseous state
mixed with other vapors and gases. No odor or color is contributed to the mixture by the
carbon disulfide.
10.2.4.2 Properties
Formula CS2
Boiling Point 46.28ºC (115F) at 760 mm Hg
Specific Gravity 2.63 for vapor with respect to air.
Auto Ignition Temperature 90ºC (194F) to 125ºC (257F) (range reported by

different sources)
Explosive Limits 1.0% to 50.0% by volume in air.
Solubility in Water 0.22 grams CS2 per 100 grams at 22ºC (72F)
Document No.:
149-RP-PR35-0003.01
MANUAL
Carbon disulfide, even at low concentrations, acts as a slight irritant to the eyes and
respiratory tract. The maximum allowable exposure over an eight hour work period is 20
ppm by volume. At concentrations greater than 20 ppm, it can be highly toxic, especially
when inhaled. Because it has no color or appreciable odor, and especially since it can
be absorbed through the skin, exposure to carbon disulfide is dangerous.
The chief toxic effect is on the central nervous system, acting as a narcotic and
anesthetic in acute poisoning, with death following from respiratory failure.
Carbon disulfide is highly dangerous when exposed to heat, flame, sparks, or friction
and is a severe explosion hazard. Note the wide explosive range under "Properties"
above.
Since carbon disulfide can be fatal if inhaled, supplied-air or oxygen respiratory

equipment of appropriate design with full-face mask should be used by all persons
entering a contaminated area.
10.2.5. Carbonyl Sulfide (Carbon Oxysulfide)
9.2.5.1 Description
At ordinary room temperature and atmospheric pressure, carbonyl sulfide is a colorless

gas with an unpleasant odor, unless it is very pure. It is also known by the name carbon
oxysulfide.
Document No.:
149-RP-PR35-0003.01
MANUAL
In the Sulfur Recovery Unit it is found in the gaseous state mixed with other vapors and
gases. No odor or color is contributed to the mixture by the carbonyl sulfide.
10.2.5.2 Properties
Formula COS
Boiling Point 50.2ºC (58ºF) at 760 mm Hg
Specific Gravity 2.07 with respect to air.
Explosive Limits 12% to 28.5% by volume in air at room

temperature.
Solubility in Water 80 cc COS per 100 grams at 14ºC (57F)
Carbonyl sulfide is severely toxic, a strong nerve poison, and can cause injury to skin or
mucous membranes with permanent physical impairment or disfigurement. Continuous
or frequent exposure to small amounts can cause death. Its toxicity is reported to be
similar to that of H2S.
Carbonyl sulfide is dangerous when exposed to heat, flame, sparks, or friction and is a
severe explosion hazard.
Since carbonyl sulfide can be painful, and/or fatal if inhaled, supplied-air or oxygen
respiratory equipment of appropriate design with full-face mask should be used by all
persons entering a contaminated area.
Document No.:
149-RP-PR35-0003.01
MANUAL
10.2.6. Ammonia
10.2.6.1 Properties
Formula NH3
Color Colorless
Odor Penetrating, intensely pungent and suffocating

odor.
Corrosive Corrosive to eye and respiratory tissues; attacks

copper, silver, zinc and their alloys; forms explosive
compounds with mercury and silver.
Specific Gravity 0.589 with respect to air
Affinity for Water One volume of water absorbs 1,150 volumes of

ammonia at standard pressure and 0oC.
Explosive limits 15% to 28% NH3 by volume in air at room

temperature
Ammonia is irritating to the eyes and mucous membranes of the respiratory tract. Signs
and symptoms of exposure are irritation of the eyes, conjunctivitis, swelling of the
eyelids, irritation of the nose and throat, coughing, dyspnoea and vomiting. Irritation of
the skin, especially if it is moist, may be experienced. Corneal ulcers have been reported
following splashing of ammonia water in the eye. Exposure to the liquid or to high
concentrations of vapor may cause severe burns or blindness. Inhalation of the fumes
may cause corrosion of mucous membranes and severe damage to the lungs. For an
eight hour work period, OSHA's standard is a maximum of 50 ppm. The American
Document No.:
149-RP-PR35-0003.01
MANUAL
Conference of Governmental Industrial Hygienists (ACGIH) recommends a maximum of

25 ppm. A concentration of 5,000 to 10,000 ppm of NH3 vapor is rapidly fatal and causes
respiratory spasm, strangulation, and asphyxia.
b. Fire and Explosion Hazards
Ammonia is a moderate fire hazard when exposed to heat or flame. It forms a moderate
explosion hazard when exposed to flame. It forms explosive compounds with silver or
mercury.
An industrial gas mask with a green canister may be used for concentrations up to 2%
and for a maximum of 15 minutes. A self-contained oxygen breathing apparatus or
supplied-air mask is preferable. Maintenance men, who must work where the ammonia
concentration is greater than 1.52.0% should wear a one-piece ventilated rubber or
neoprene suit. This suit is sealed at the face, wrists and ankles. Goggles and gloves
should be worn when working around ammonia.
a. Inhalation
Remove patient to fresh air or to a well ventilated room immediately. If breathing has
stopped, start artificial respiration at once and continue until the patient is conscious. An
approved resuscitator with oxygen should be used as soon as it is available. Keep the
patient warm, but not hot, and on his back with his feet slightly elevated. Use a stretcher
to move him. Do not give anything by mouth to an unconscious patient.
b. Contact with Eyes
Irrigate the eyes immediately with large quantities of water for at least 10 minutes. Hold
the eyelids apart during the irrigation. Be sure to take the patient to a physician or an eye
specialist for further treatment. Two drops of 0.5% Pontocaine solution may be applied
to each eye if the patient is in great pain after irrigation of his eyes and is unable to see a
physician within a short period of time.
c. Contact with Skin
Wash contact area with plenty of water. Take patient to physician for treatment.
Document No.:
149-RP-PR35-0003.01
MANUAL
d. Nose and Throat Burns
Gargle thoroughly with a 2% solution of boric acid (or plain water). The patient should
draw up a 2% solution of boric acid through his nose. Drink large quantities of water,
milk or lemonade.
10.2.7. H2S & NH3 Mixtures
In addition to the normal hazards of the individual compounds, there exist other hazards when
these components are mixed. These compounds will spontaneously react with each other
without presence of any catalyst forming insoluble ammonium polysulfide salts (NH4Sx). These
salts tend to precipitate in equipment such as knock-out drums, exchangers, etc. as well as the
pipelines. These salts will plug meter leads, sample connections, exchanger tubes and in
severe cases, the main process lines.
The amount of reaction depends on the relative composition of each component in the overall
stream. The greatest potential for reaction occurs in a 50-50 mixture of ammonia (NH3) and
hydrogen sulfide (H2S). However, the reaction does occur readily at lower relative
concentrations of NH3.
The reaction occurs generally at low temperatures (<82C) and can be prevented if the process
temperature remains relatively warm. Experience has indicated that if the process stream
remains at or above 82°C, the insoluble salt formation can be effectively eliminated. This
temperature limit is based on system pressures normally encountered in sour water stripper
overhead streams, such as 0.70-0.84 psig. Increased system pressure enhances the possibility
of the NH3-H2S reaction and thus a higher temperature (>82C) would be required to prevent the
reaction.
Experience has also indicated that the reaction to form the solid salts is basically irreversible.
Once the salts have precipitated, increasing the system temperature does not eliminate the
plugging problem. Temperatures as high as 110C have been used in an effort to eliminate the
solids, but this has been unsuccessful. However, if the salts have precipitated, they can
successfully be washed away with water. Unfortunately this "water washing" step usually
requires a unit shutdown, thus the formation of these salts should be prevented.
10.2.8. Diethanolamine (DEA)
Refer to Material Safety Data Sheets (MSDS) obtained from selected DEA supplier.
10.2.9. Carbon
Refer to Material Safety Data Sheets (MSDS) obtained from selected DEA supplier.

Supervisory Operating Manual: UNIT NO.: 07 (Amine 2) Amine Regeneration Unit Cartagena Refinery Expansion Project

Uploaded by

Copyright:

Available Formats

Supervisory Operating Manual: UNIT NO.: 07 (Amine 2) Amine Regeneration Unit Cartagena Refinery Expansion Project

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Supervisory Operating Manual: UNIT NO.: 07 (Amine 2) Amine Regeneration Unit Cartagena Refinery Expansion Project

Uploaded by

Copyright:

Available Formats

What is the purpose of the amine regeneration unit?

What is the purpose of the amine regeneration unit?

What are the main components of the amine regeneration unit?

What are the main components of the amine regeneration unit?

SUPERVISORY OPERATING MANUAL

UNIT NO.: 07 (Amine 2)

CB&I CONTRACT NO. 166004

0a 9-Dec-11 Issued for Information ELP AMC AMC

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 2 of 113

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 3 of 113

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 4 of 113

1.1 CONFIDENTIAL NOTE

1.2 PURPOSE OF THE UNIT

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 5 of 113

1.3 DESIGN BASIS

Case B1 Case C/D

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 6 of 113

1.4 PRODUCT CHARACTERISTICS

1.5 SCOPE OF MANUAL

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 7 of 113

1.1 PROCESS CHEMISTRY

1.2 PROCESS FLOW DESCRIPTION

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 8 of 113

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 9 of 113

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 10 of 113

2 MECHANICAL DESCRIPTION (NEW EQUIPMENT ONLY)

3.1 HEAT TRANSFER EQUIPMENT

3.1.1 SU-E-2008 A/B LEAN AMINE COOLER

3.1.1.1 Principle Reference Drawings

P&ID: 4-07-EB-003 Sheet 4

Cools lean amine before routing to users

3.1.1.3 Design Data

Design duty: 10.6 MM BTU/hr plus 10%

3.1.1.4 Operating Conditions

Tube (Cooling Water): Inlet: 70 psig @ 90 °F

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 11 of 113

3.1.2 SU-E-2009 LIQUID EJECTOR MOTIVE LIQUID COOLER

3.1.2.1 Principle Reference Drawings

P&ID: 4-07-EB-004 Sheet 3

3.1.2.3 Design Data

Design duty: 0.9 MM BTU/hr plus 10%

3.1.2.4 Operating Conditions

Tube (Cooling Water): Inlet: 70 psig @ 90 °F

AMINE REGENERATION UNIT, Amine 2 Date: 15-Mar-12

Page: Page 12 of 113

3.2 PRESSURE VESSELS

3.2.1 SU-D-2007 RICH AMINE FLASH DRUM

3.2.1.1 Principle Reference Drawings

P&ID: 4-07-EB-003 Sheet 2