JOB No. DOC. No. REV.

Project Specification 0-0800 S-801-1230-001 3

DATE 07 -OCT- 1998 SHEET 1 OF 105
PREP’D T. TAKEDA
CHK’D N.A
APP’D T. KIMURA

OPERATING MANUAL

FOR

Unit: 801

KEROSENE MEROX PROCESS UNIT

DISTRIBUTION
PARCO KPO 1
IPMT 2
BKW
PARCO SITE
PMT 1
P-CONT
CONST
ENG 1

PROCESS 2 PAK-ARAB REFINERY LIMITED

PIPING
CIVIL MID-COUNTRY REFINERY PROJECT
INST
ELEC
ROTARY
FIRE MAHMOOD KOT, PAKISTAN
ACOUSTIC
EQUIP
PAINT/ INSU
PKG(PK)
PKG(SH)
COMB
BLDG/HVAC
OPERAT 1
LABO
LEGAL INDEX
PPM
PURCH 1-1
PURCH 1-2
PURCH 1-3
PURCH 2-1 REV. DATE PAGE DESCRIPTION PREP’D CHK’D APP’D
PURCH 2-2-E
PURCH 2-2-I 0 07-OCT-98 All FOR REVIEW T. TAKEDA N.A. T. KIMURA
EXPED’G
SHIPPING 3 16-APR-99 As Marked ISSUED FOR CONSTRUCTION(REVIEWED WITH X-JY/PY-3801 AND UPDATED) T. TAKEDA N.A. T. KIMURA
QA
QC
JPC

MARUBENI
SITE
TIC
JUS
JEU
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TABLE OF CONTENTS
PAGE

1. GENERAL DESCRIPTION ············································································ 7

1.1. PLANT DUTY ···························································································· 7

1.2. DISCUSSION OF PROCESS ············································································ 7
1.2.1. Merox Reactions ·················································································· 7
1.2.2. Sweetening Chemistry ········································································· 8
1.3. DESIGN BASIS FOR FEED AND PRODUCTS····················································· 10
1.3.1. Feed Properties ················································································· 10
1.3.2. Product Specification ········································································· 11
1.3.3. Design Considerations ········································································ 16
1.4. MATERIAL BALANCE / B.L. CONDITIONS ······················································ 16
1.4.1. Battery Limit ( B.L. ) Conditions ·························································· 16
1.4.2. Material Balance of Kerosene Merox Process Unit ·································· 18
1.5. UTILITIES AND CHEMICAL REQUIREMENTS ·················································· 19
1.5.1. Utilities Requirements ······································································· 19
1.5.2. Chemical Requirements······································································ 19

2. OPERATING CONDITIONS AND CONTROLS ·············································· 20

2.1. DISCUSSION OF PROCESS VARIABLES ·························································· 20

2.1.1. Pretreatment Section ········································································· 24
2.1.2. Sweetening Section ············································································ 25
2.1.3. Post Treatment Section ······································································ 28
2.2. PROCESS FLOW AND CONTROL··································································· 29
2.2.1. Description of Process Flow ································································· 29
2.2.2. Control Flow Plan ·············································································· 32

3. EMERGENCY EQUIPMENT ······································································· 35

3.1. SAFETY VALVES ······················································································ 35

3.1.1. Summary of Flare Loads····································································· 35
3.2. CAR SEALED VALVES ················································································ 35
3.3. REMOTE OPERATING VALVES ···································································· 37
3.4. INSTRUMENT ALARMS ·············································································· 37
3.5. INSTRUMENT TRIP SETTINGS ····································································· 39
3.6. PROCEDURES FOR SETTING PROTECTIVE RELAYS ··········································· 40

4. PREPARING THE UNIT FOR PRE-COMMISSIONING ·································· 42

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4.1 PRE-COMMISSIONING ·············································································· 42
4.2. COMMISSIONING OF UTILITIES ·································································· 42
4.3. PRESSURE TESTING ················································································· 43
4.4. FLUSHING OUT ······················································································· 44
4.5. ACID CLEANING OF RECIPROCATING COMPRESSOR LINES ······························· 46
4.6. INSPECTION AND RUN-IN OF PUMPS AND FANS ············································· 46
4.7. LEAK TEST····························································································· 48
4.8. INSPECTION AND RUN-IN OF RECIPROCATING COMPRESSOR ···························· 49
4.9. INSPECTION AND RUN-IN OF CENTRIFUGAL COMPRESSOR······························· 49
4.10. LOADING INTERNAL MATERIAL REQUIRED FOR ABSORBERS, VESSELS, PACKED
COLUMNS, ETC. ····························································································· 49
4.10.1. Preparation of 10o Be and 3o Be caustic solutions ·································· 49
4.11. DRYING OUT FIRED HEATER ···································································· 50
4.12. DRYING OUT REACTOR SECTION ······························································· 50
4.13. PREPARING REACTORS ··········································································· 50
4.14. LOADING CATALYST ··············································································· 50
4.15. CHEMICAL BOIL-OUT OF STEAM GENERATION FACILITIES ······························ 50
4.16. PURGING AND GAS BLANKETING ······························································· 50
4.17. PRE-COMMISSIONING CHECK LIST ····························································· 52

5. COMMISSIONING ····················································································· 54

5.1. GENERAL OVERALL COMMISSIONING PLAN. ·················································· 54

5.2. DETAILED STEP-BY-STEP PROCEDURE ························································· 54
5.2.1. Preparation for start-up······································································ 54
5.2.2. Nitrogen Pressure Up / Tightness Test ················································· 55
5.2.3. Unit Line up ····················································································· 55
5.2.4. Introduction of Feed ··········································································· 56
5.2.5. Final Plant Adjustment ······································································ 56
5.3. SPECIAL PRECAUTIONS ············································································ 57

6. NORMAL START-UP AND SHUTDOWN ······················································ 58

6.1. NORMAL START-UP AFTER PROLONGED SHUTDOWN ······································· 58

6.2. NORMAL START-UP AFTER SHORT SHUTDOWN ··············································· 58
6.3. NORMAL OPERATIONS ·············································································· 58
6.3.1. Adjustment of Operating Parameters ··················································· 58
6.3.2. Operating Guidelines ········································································· 61
6.3.3. Catalyst Deactivation ········································································· 61
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6.4. ROUTINE OPERATIONS ············································································· 63
6.4.1. Special Procedures ············································································ 63
6.4.2. Trouble Shooting ··············································································· 73
6.5. GENERAL OVERALL SHUTDOWN PLAN ························································· 75
6.6. DETAILED STEP-BY-STEP SHUTDOWN PROCEDURE ········································· 76
6.7. BLANKING OFF ······················································································· 76
6.8. OPENING EQUIPMENT ·············································································· 77
6.9. SPECIAL PRECAUTIONS ············································································ 78
6.9.1. Safely Entering A Contaminated Atmosphere ········································ 78

7. EMERGENCY SHUTDOWN ········································································ 80

7.1. GENERAL INSTRUCTIONS ·········································································· 80

7.2. FIRE ····································································································· 80
7.3. POWER FAILURE ····················································································· 81
7.4. INSTRUMENT AIR FAILURE ········································································ 81
7.5. LP STEAM FAILURE ················································································· 81
7.6. WATER FAILURE ····················································································· 82
7.6.1. Cold Condensate failure ····································································· 82
7.6.2. Cooling Water failure ········································································· 82
7.7. FEEDSTOCK FAILURE ··············································································· 82
7.8. EQUIPMENT FAILURE··············································································· 82

8. MAJOR EQUIPMENT AND ITS SERVICE ···················································· 83

8.1. SUMMARY TABLES ··················································································· 83

8.2. TOWER SUMMARY ···················································································· 83
8.3. DRUM SUMMARY ····················································································· 83
8.3.1. Electrostatic Coalescer Prewash ( 801-ME7 ) ········································· 83
8.3.2. Caustic Settler ( 801-V1 ) ···································································· 84
8.3.3. Wash Water ( 801-V3 ) ······································································· 85
8.3.4. Salt Filter ( 801-V4 ) ·········································································· 86
8.3.5. Clay Filter ( 801-V5 )·········································································· 87
8.4. REACTOR SUMMARY ················································································· 90
8.4.1. Reactor ( 801-R1 ) ·············································································· 90
8.5. FIRED HEATER SUMMARY·········································································· 91
8.6. EXCHANGER SUMMARY············································································· 91
8.7. PUMP SUMMARY ····················································································· 91
8.7.1. Caustic Transfer Pumps ( 801-P1A/B ) ·················································· 91
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8.7.2. Caustic Injection Pumps ( 801-P2A/B ) ·················································· 91
8.7.3. Merox Plus Injection Pumps ( 801-P3A/B ) ············································ 91
8.7.4. Circulation Pumps ( 801-P4A/B )·························································· 92
8.7.5. Wash Water Pump ( 801-P5 ) ······························································ 92
8.8. COMPRESSOR SUMMARY ··········································································· 92
8.9. SPECIAL EQUIPMENT SUMMARY ································································· 92
8.10. LIST OF INSTRUMENTS ··········································································· 92
8.11. SUMMARY OF ALL EQUIPMENT’S DRIVERS ··················································· 92
8.12. CONTROL VALVES·················································································· 93
8.13. FIRED HEATER······················································································ 93
8.14. MISCELLANEOUS ··················································································· 93

9. FLOW PLANS AND PLOT PLAN ································································· 94

9.1. PFD, MSD AND P&IDS ············································································ 94

9.2. DESIGN ENGINEERING, UTILITY AND SAFETY FLOW PLANS ······························ 94
9.3. PLOT PLAN ···························································································· 94
9.4. SAFETY SHUTDOWN FUNCTION CHARTS ······················································· 94

10. SAFETY ·································································································· 95

10.1. EMERGENCY FIRE PLAN ·········································································· 96

10.2. FIRE FIGHTING AND PROTECTIVE EQUIPMENT ············································· 96
10.3. FIRE PROTECTION ················································································· 97
10.4. MAINTENANCE OF EQUIPMENT AND HOUSEKEEPING ···································· 98
10.5. REPAIR WORK ······················································································· 99
10.6. THERMAL EXPANSION IN EXCHANGERS ······················································ 99
10.7. WITHDRAWAL OF SAMPLES ····································································· 100
10.8. SAFE HANDLING OF VOLATILE AND TOXIC MATERIALS INCLUDING CATALYST ···· 100
10.8.1. Respiratory Protection ····································································· 100
10.8.2. Breathing Apparatus ( B. A. ) ··························································· 101
10.8.3. Corrosive Materials ········································································· 102
10.8.4. Poisonous Materials ········································································ 102
10.9. PREPARING FOR ENTERING PROCESS EQUIPMENT ······································· 105
10.10. OPENING EQUIPMENT ·········································································· 106
10.11. WORKING IN COLUMNS OR VESSELS························································ 107
10.12. ENTERING TANKS, DRUMS OR OTHER VESSELS ·········································· 107
10.13. PROCEDURE FOR REMOVING SAFETY VALVES ············································ 108
10.14. WORK PERMIT PROCEDURE AND WORK PERMIT FORMAT ····························· 108
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10.15. OPERATION NOTES RELATING TO HAZOP REVIEW ····································· 108
10.16. MATERIAL SAFETY DATA SHEET ( MSDS ) OF ALL THE CHEMICALS, CATALYSTS,
ETC. ·········································································································· 109

11. MISCELLANEOUS·················································································· 110

11.1. CONVERSION TABLES ············································································ 110

11.2. GENERAL PRE-START UP PROCEDURES ····················································· 110
11.3. OVERALL START-UP AND SHUTDOWN OUTLINES ·········································· 110
11.4. OFFSITE SYSTEMS ················································································· 111
11.5. CATALYST AND CHEMICAL LOADING / UNLOADING ····································· 111
11.6. CATALYST AND CHEMICAL REQUIREMENTS ··············································· 111
11.7. ANALYTICAL PLAN ················································································ 111
11.7.1. General Procedure ·········································································· 111
11.7.2. Analytical Schedule ········································································· 115

LIST OF ATTACHMENT
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1. GENERAL DESCRIPTION

1.1. Plant Duty

The processing capability of the Kerosene Merox Process Unit shall be 20,000
BPD ( 132.49 m3/hr ) of kerosene to achieve a jet fuel product with less than 10
wppm mercaptan and less than 1 wppm sodium. The processing objective is to
produce JP-1 ( Jet A-1 ), kerosene as per the Pakistan specifications, and as
blending component for JP-4.

1.2. Discussion of Process

To fully understand the Merox process and how it can be applied to such a broad
range of treating problems, it is necessary to review the basic chemical reaction of
the process and how it is applied in a variety of ways. UOP may have been remiss
in using the name “Merox” to designate a variety of applications of a single
catalyzed chemical reaction. The use of a single name to designate what may
appear to be a multiplicity of processes has unfortunately been the cause of some
confusion in understanding the various applications of the process.

1.2.1. Merox Reactions

The name “Merox” originates from the function of the process itself; namely the
conversion of mercaptans by oxidation.
MERcaptan
OXidation
The word “mercaptan” is a descriptive name applied over 140 years ago to organic
compounds with a sulphydryl function ( -SH ) and derived from the Latin
mercurium captans, due to their mercury seizing properties. Today’s literature,
however, assigns the word “thiol” for this functional group.

In the common system used by the petroleum industry, mercaptans are named
after their analogous alcohol counterparts. Thus, CH3SH, by the common system,
is methyl mercaptan just as one would name an alcohol having the formula
CH3OH methyl alcohol; the strict formal name is “methanethiol”. Likewise,
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n-butyl mercaptan becomes 1-butanethiol, t-butyl mercaptan becomes
2-methyl-2-propanethiol. The aryl mercaptans are commonly called thiophenols,
while in the formal systems used by Chemical Abstracts, these compounds are
benzenethiol, toluenethiol, etc. this discussion uses the common mercaptan
terminology as practiced in the petroleum industry.
The Merox process in all its applications is based on the ability of an
organometallic catalyst to accelerate the oxidation of mercaptans to disulfides at
or near ambient temperatures and pressures. Oxygen is supplied from the
atmosphere. The reaction will proceed only in an alkaline environment. That
overall reaction can be written:
RSH + ¼ O2  ½ RSSR + ½ H2O
R is a hydrocarbon chain which may be straight, branched, or cyclic. These chains
may be saturated or unsaturated. In its various aspects, under the proper
circumstances, and depending upon the results desired, it is applicable to the
treatment of stocks boiling up to 345 oC endpoint.
Sweetening occurs when a hydrocarbon containing mercaptans is brought into
contact with caustic soda solution, air, and the catalyst to convert the mercaptans
to oil soluble disulfides without changing the sulfur content of the hydrocarbon.

1.2.2. Sweetening Chemistry

Sweetening is applied to distillates containing mercaptans which cannot be more

or less completely removed by caustic extraction. Sweetening converts the
mercaptans to disulfides which remain in the distillate. Sweetening takes place
by contacting the mercaptan containing distillate with soda solution, air, and
catalyst. The overall sweetening reaction is given by the following equation:
2 R’SH + 2 RSH + O2  2 R’SSR + 2 H2O
R and R’ represent hydrocarbon chains. In most petroleum fractions, there will be
a mixture of mercaptans to the extent that the R chain might have 1,2,3,…10 or
more carbon atoms in the chain. When this reaction occurs, two different
mercaptans might enter the reaction. This is indicated by showing R and R’ in the
reaction.
This reaction occurs spontaneously, but a very slow rate, whenever any sour
mercaptan bearing distillate is exposed to atmospheric oxygen. It is the purpose
of a sweetening process to speed up this reaction. Most sweetening processes do
this indirectly by using supplemental chemical reagents.
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Figure 1.1
Oxidation of Mercaptans with Air and Caustic

No

Mercapta

With Merox
Catalyst

Time

In about 1958, UOP introduced the Merox process which directly speeds up this
reaction at or near ambient temperature by using a unique catalyst dispersed in
an alkaline environment ( Figure 1.1 ).
It is believed on the basis of UOP studies, that the mercaptan, or at least the thiol
( -SH ) functional group, first transfer to the aqueous alkaline phase ( Figure 1.2 )
and then combines with the catalyst. The simultaneous presence of oxygen causes
this mercaptan-catalyst complex to oxidize, yielding a disulfide molecule and
water.

Figure 1.2
Mercaptide at Interface

OIL PHASE

S-
N
O

H
O

Aqueous
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The purpose of the caustic is twofold:

 To transfer the mercaptan, or at least the thiol portion of the mercaptan, to
the aqueous phase, and
 To supply the alkaline environment needed for the reaction to proceed in the
direction desired.
This system works efficiently for all the lower molecular weight mercaptans
which are partially soluble in caustic soda solution.
Difficulties can be encountered with higher boiling stocks, such as kerosene and
jet fuel, that contain mercaptans of such high molecular weight that they are not
measurably soluble in caustic solution. Fortunately, however, the thiol function
( -SH ) appears to retain its solubility in the aqueous phase. But since the
mercaptan molecule itself may not be soluble and exhibits a very low degree of
dissociation or ionization, the sweetening reaction must occur at the oil/water
interface.
The most important point to remember, and the point that makes the Merox
process unique, is that the Merox reaction occurs in the aqueous phase. Most of
the other mercaptan oxidation processes utilize oxidation reactions which occur
in the oil phase. An oil phase reaction is much less desirable because there are
many competing oxidation reactions which can occur in the oil phase to leave
contaminants in the product.

1.3. Design Basis for Feed and Products

1.3.1. Feed Properties

The feed to the Kerosene Merox Process Unit is the kerosene from the Kerosene
Stripper at the Crude Distillation Process Unit.

Property Value
Designation Kerosene
Feed Source Crude Distillation Process Unit
Feed rate, BPD 20,000 ( 132.49 m3/hr )
Turndown Rate, 10,000 ( 66.245 m3/hr )
BPD
Crude Source(s) Arabian Light or blend of Murban and Upper
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Zakum

The following are the expected feed qualities.

Property Values Test Method

TBP Cut Range 150 - 232 oC ---
SpGr ( 15/4 oC ) 0.739 ASTM D1298
Mercaptan 190 wt ppm (max.) UOP 163
Acidity 0.02 mgKOH/g (max.) ASTM D3242
H2S nil UOP 163

1.3.2. Product Specification

The Merox-treated kerosene product shall be routed to storage and shall meet the
specifications for JP-1 ( Jet A-1 ) Aviation Turbine Fuel, JP-4 Aviation Turbine
Fuel(product blended with light/heavy naphtha) and Kerosene as shown in the
following tables:

Table: 1.1 Specification for Aviation Turbine Fuel Grade JP-4 ( MIL-T-5624L )

Property Value Min/Ma Test Method

x
1 Aromatics, vol % 25 max ASTM D-1319
2 Olefins, vol % 5 max ASTM D-1319
3 Mercaptan Sulfur, wt % 0.001 max ASTM D-3227
4 Total Sulfur, wt % 0.4 max ASTM D-1226
or D-2622
5 Distillation IBP, oC Report - ASTM D-86
10 vol% Distilled, oC Report - ASTM D-86
20 vol% Distilled, oC 145 max ASTM D-86
50 vol% Distilled, oC 190 max ASTM D-86
90 vol% Distilled, oC 245 max ASTM D-86
Distillation End point, oC 270 max ASTM D-86
Distillation Residue, vol % 1.5 max ASTM D-86
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Distillation Loss, vol % 1.5 max ASTM D-86

6 Density @ 15 oC, kg/m3 751 - - ASTM D-1298
802
7 Reid Vapor Pressure, 37.8oC, 0.14 - - ASTM D-323
kg/cm2 0.21 or D-2551
8 Freezing Point, oC -58 max ASTM D-2386
9 Total Acid Number, mg KOH/g 0.015 max ASTM D-3242
10 Net Calorific Value, kcal/kg 10,230 min ASTMD-240 or
or Aniline Gravity Product 5,250 min D-2382 or
D-3338
ASTM D-1405
11 Smoke Point, mm 20 min ASTM D-1322
or Hydrogen Content, wt% 13.6 min ASTM D-1018
or
D-3343 or
D-3701
12 Copper Strip Corrosion, 2hr @ lb max ASTM D-130
100oC
13 Thermal Stability: 25 max ASTM D-3241
Change in Pressure Drop,
mmHg 3 max
Preheater Deposit Code
14 Existent Gum, mg/100ml 7.0 max ASTM D-381
15 Particulate Matter, mg/liter 1.0 max ASTM D-2276
16 Filtration Time, minutes 10 max ASTM D-2276
17 Water Reaction Interface lb max ASTM D-1094
Rating
18 Water Separation Index, 85* min ASTM D-2550
Modified 70** min
19 Fuel System Icing Inhibitor, 0.10 - -
vol% 0.15
20 Color, Saybolt Report - ASTM D-156
21 Electrical Conductivity, μS/m 200 - - ASTMD-2624
600 or
D-3114
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* - with additives except corrosion inhibitor and ASA-3.
** - with all additives except ASA-3.
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Table: 1.2 Specification for Aviation Turbine Fuel Grade JP-1 ( Jet A-1 ).

Property Value Min/Max Test Method

1 Appearance Visually clear, bright, free from solid
matter and undissolved water
2 Aromatics, vol % 22 max ASTM
D-13
19
3 Olefins, vol % 5 max ASTM
D-13
19
4 Net Calorific Value, kcal/kg, 10,230 min ASTM
D-23
or Aniline Gravity Product 4,800 min 82
or D-1405
ASTM
D-12
98
or D-611
5 Copper Content, mg/kg 150 max IP-225
6 Copper Strip Corrosion, 2hr @ 100 No. 1 max ASTM D-130
oC

7 Silver Strip Corrosion, 4hr @ 50 oC No. 1 max IP-227

8 Distillation IBP, oC Report - ASTM D-86
10 vol% Distilled, oC 204 max ASTM D-86
20 vol% Distilled, oC Report - ASTM D-86
50 vol% Distilled, oC Report - ASTM D-86
90 vol% Distilled, oC Report - ASTM D-86
Distillation End point, oC 300 max ASTM D-86
Distillation Residue, vol % 1.5 max ASTM D-86
Distillation Loss, vol % 1.5 max ASTM D-86
9 Electrical Conductivity, μS/m 50 - 450 - ASTM A-2624
10 Existent Gum, mg/100ml 7.0 max ASTM D-381
11 Flash Point, oC 38 min IP-170
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12 Freezing Point, oC -47 max ASTM

D-23
86
13 Smoke Point, mm 19 min ASTM
D-13
22
14 Specific Gravity, 15.6/15.6 oC 0.775 min ASTM
0.830 max D-12
98
15 Mercaptan Sulfur, wt % 0.001 max ASTM
D-13
or Dr. Test Negative - 23
or D-3227
ASTM D-484
16 Total Sulfur, wt % 0.15 max ASTM
D-12
66
17 Thermal Stability ( JFTOT ) ASTM
Tube Rating ( visual ) <3 - D-32
Filter Pressure Difference, mm/Hg 25 max 41

18 Total Acidity, mg KOH/g 0.015 max ASTM

D-32
42
19 Viscosity @ -20 oC, cSt 8.0 max ASTM D-445
20 Water Reaction ASTM
Interface Rating lb max D-1094
Separation Rating 2 max
21 Water Separometer Index 85 min ASTM
Modified 70* min D-2550
* - when ASA-3 has been added.

Table : 1.3 Specification for Kerosene *

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Property Value Min/Max Test Method

Specific Gravity, 15.6/15.6 oC 0.820 max ASTM D-1298
Distillation: 20% Recovery, oC 200 max ASTM D-86
Distillation: End point, oC 300 max ASTM D-86
Color ( Saybolt ) +20 min ASTM D-156
Flash Point, oC 35 min IP-170
Smoke Point, mm 22 min ASTM D-1322
Wick Characteristic, mg/kg 20 max ASTM D-187
Total Sulfur, wt % 0.20 max ASTM D-1266
Copper Corrosion 1 max ASTM D-130
Mercaptan Sulfur, wt ppm 10 max ASTM D-1323
Odor Marketable
* - the specification of kerosene will also be the same as the specifications for JP-1
( Jet A-1 ).

1.3.3. Design Considerations

1. Injection facilities for Merox Plus, a high activity catalyst promoter, will be
specified in order to increase catalyst life.
2. Equipment design pressure will typically be based on pump shut-in pressure
to avoid a liquid relief case.
3. The reactor occasionally requires a hot water wash ( at 93 oC ) to restore the
activity of the Merox catalyst. The water used for this procedure will be
cooled with quench water before leaving the Kerosene Merox Process Unit.
4. Provisions will be incorporated in the design to facilitate the conversion of the
Kerosene Merox Process Unit to a caustic-free operation.

1.4. Material Balance / B.L. Conditions

1.4.1. Battery Limit ( B.L. ) Conditions

Fluid Origin / Destination Available Temperature

Pressure ( oC )
( kg/cm2G )
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1) Incomings
Raw Kerosene Crude Unit 8.44 40
25o Be caustic 900-TK1A/B 2.0 40
Cold Condensate Condensate header 3.1 52.5

2) Outcomings
Treated Kerosene Tankage and Blending 3.52 40
System
Spent Caustic 930-TK5 3.5 40
10o Be caustic Caustic Header 11.7 ( min ) 40
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1.4.2. Material Balance of Kerosene Merox Process Unit

Stream Number* 3 21 72 129

Stream Name ( FEED ) Kerosene Pre-washed Injected Compressed
from Crude kerosene to caustic to air to Mixer
Unit Mixer Prewash
H2O ,Kg mol/h - - 8.92 -
O2 ,Kg mol/h - - - 0.31
N2 ,Kg mol/h - - - 1.17
HCBN FD,Kg mol/h 669.72 669.72 - -
RSH ,Kg mol/h 0.62 0.62 - -
RSSR ,Kg mol/h - - - -
NaOH ,Kg mol/h - - 0.07 -

Total Mole Flow, 670.34 670.34 8.99 1.48

Kg-mol/hr
Weight Flow, kg/hr 105,100 105,100 164 43
Mole weight, kg/kg mole 156.79 156.79 18.19 28.85
Liq Vol Flow, Std m3/hr 132.49 132.49 0.16 0
Liq Density, kg/m3 793 793 1015 0
Vap Vol Flow, m3/hr - - - 33
( Norm )
Vap Density, kg/m3 - - - 1.3
( Norm )
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Stream Number* 38 74
Stream Name ( PRODUCT ) Treated Kerosene to Pre-washed
Tankage kerosene
to Mixer
H2O ,Kg mol/h - -
O2 ,Kg mol/h 0.16 -
N2 ,Kg mol/h 1.17 -
HCBN FD,Kg mol/h 669.72 -
RSH ,Kg mol/h - -
RSSR ,Kg mol/h 0.31 -
NaOH ,Kg mol/h - 0.07

Total Mole Flow, Kg-mol/hr 671.36 8.99

Weight Flow, kg/hr 105,140 164
Mole weight, kg/kg mole 156.61 18.19
Liq Vol Flow, Std m3/hr 132.53 0.16
Liq Density, kg/m3 793 1,015
Vap Vol Flow, m3/hr ( Norm ) - -
Vap Density, kg/m3 ( Norm ) - -
Refer to Attachment 9.1 ( PFD of the Kerosene Merox Process Unit ) for details.

1.5. Utilities and Chemical Requirements

1.5.1. Utilities Requirements

Refer to Attachment 1.1( Utility Summary of the Kerosene Merox Process Unit,
Doc. No. S-801-1223-501 ) for details.

1.5.2. Chemical Requirements

Refer to Attachment 1.2( Catalyst and Chemical Summary of the Kerosene Merox
Process Unit, Doc. No. S-801-1223-502 ) for details.
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2. OPERATING CONDITIONS AND CONTROLS

2.1. Discussion of Process Variables

The purpose of this section is to discuss the major Merox process variables and
their effect on performance. Specific emphasis will be placed on identifying the
optimum operating conditions. Although feedstock quality is obviously a variable,
it will not be discussed here. Merox operators generally have little, if any, control
over the feedstock.
The following represent the five primary process variables. Each will be discussed
as an independent with all others held constant.
C atalyst
O xygen
A lkalinity
C ontact
H eat

Catalyst Concentration and Addition

UOP Merox No. 8 pre-impregnated catalyst may be used for this unit. A special
catalyst promoter, Merox Plus, is continuously injected into the kerosene
upstream of the reactor. The rate of addition of Merox Plus is the only controllable
variable of the catalyst concentration. Alternatively, charcoal may be used and
field impregnated using UOP Merox FB Reagent. The charcoal should be
impregnated with 1.4 kilograms of UOP Merox FB Reagent per cubic meter of
charcoal. Over the course of a run, catalyst activity will gradually decline. When
deactivation reaches an intolerable level, the reactivation with additional
catalyst should be conducted.

Oxygen Injection
Oxygen is supplied to all versions of the Merox process in the form of compressed
atmospheric air. The stoichiometric, or theoretical, amount of oxygen necessary is
0.25 kilogram per kilogram of mercaptan sulfur. One cubic meter of atmospheric
air at normal conditions of temperature and pressure contains about 0.30
kilogram of oxygen, therefore, about 0.84 Nm3 ( normal cubic meter ) of air is
needed for each kilogram of mercaptan sulfur to be oxidized . It is of course,
necessary to have at least a slight excess of oxygen present but it is always
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recommended to keep the excess to a minimum. The amount of excess air
injection necessary is highly dependent upon the individual feedstock, but
normally ranges between 1.2 to 2.0 times the theoretical requirement. Thus, a
good initial injection rate at 1.5 times theoretical may be calculated from the
formula below:
( Air ) = 1.5 ( K ) ( Feed rate ) ( S.G. ) ( RSH ) / ( 10,000 )
where :
Air = Air injection rate, Nm3/hr
K = 8.35 ( constant )
Feed Rate = Feed flow rate, m3/hr
S.G. = Specific gravity @15.5 oC
RSH = Mercaptan sulfur, wt ppm

Alkalinity
Alkalinity is needed to selectively drive the mercaptan oxidation reaction.
Alkalinity is provided by aqueous sodium hydroxide, or caustic, solution.
Caustic has the ability to bring the thiol ( -SH ) end of the mercaptan molecule
into contact with the catalyst. This ability increases with increasing caustic
strength. However, the ability to extract other impurities also increases. For this
reason 10o Baume ( 6.8 wt% ) caustic is considered an optimum.
For fixed bed sweetening, it is not necessary, or desirable, to keep caustic
circulating over the catalyst at all times. Caustic resaturation should be
conducted twice per week at the beginning of the run. As the catalytic activity
declines, there will be a need for more and more frequent resaturation of the
catalyst with caustic. Finally, at the time of imminent catalyst deactivation, even
continuous caustic circulation will no longer give a product of satisfactorily low
mercaptan content.
The fixed bed catalyst absorbs trace amounts present of any high molecular
weight materials from the hydrocarbon. This adsorbed material interferes with
access to the catalyst sites and is believed to be primary responsible for the
decline in catalytic activity. When the catalyst is resaturated with caustic, some
of this adsorbed material will be washed off the catalyst.

Contact
Contact may be defined as the intimacy of mixing of the reactants. Contact is
accomplished by one of several means. Contact can be characterized by duration
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of mixing time, by volumetric ratio of reactants, or by differential pressure which
implies degree of dispersion. With a fixed flow restriction, the differential
pressure is directly related to the linear velocity so that velocity is often taken to
be the process variable.
The primary source of contact in a fixed bed unit is the charcoal bed itself. The
porous structure of the charcoal provides the vast interfacial surface area
necessary for contact between hydrocarbon, caustic, and catalyst. The variable
used to characterize contact is residence time in the charcoal bed.
Residence time is often expressed in terms of volume of feed per hour per volume
of catalyst bed; the common term for this is liquid hourly space velocity, LHSV. As
residence time increases ( LHSV decreases ), mercaptan conversion increases
( Figure 2.1 ).
Figure 2.1
Sweetening

Mercapta

Residence time

As the catalyst bed accumulates running time, the charcoal pores tend to plug
and become blinded by extremely heavy hydrocarbon molecules. This reduces
contact and is largely the cause of fixed bed deactivation. Fixed bed deactivation
results in higher mercaptan content in the product which will not respond to
corrective action. As a result, reduced feed rates for lower LHSV or catalyst bed
reactivation will be required.

Heat ( Temperature )
Fixed bed sweetening is favored by higher temperature. Increasing the
hydrocarbon feed temperature increase the rate of mercaptan conversion.
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However, increasing the temperature will also enhance other oxidation reactions
which may be undesirable because of color deterioration, gum precursor
formation, and premature catalyst bed deactivation.
Therefore, the feed temperature should be kept as low as possible while still
maintaining the desired degree of mercaptan conversion; normally this is in the
range of 38o to 50 oC. Temperature is also limited by storage considerations such
as flash point or vapor losses. Feed temperature in excess of 60 oC for long
periods should be avoided because of metallurgical considerations.

Feed Quality
Impurities will be defined as non-hydrocarbon constituents, although they may
be, and quite often are, attached to a hydrocarbon molecule. These constituents
are found in rather low concentrations relative to the hydrocarbon constituents.
The word “trace” in concentrations is a misnomer, because it means different
things to different people. For example, in one case a refiner stated that a certain
LPG stream contained only a “trace” of mercaptan and consequently no treating
was provided for its removal. Subsequently, the LPG was found to contain about
0.1 % sulfur as mercaptan which is considered a rather high concentration for
most uses.
The word “impurity” is also a misnomer because this word implies something
undesirable. Not everything that one may want to remove, or modify, can be
considered undesirable. Sometimes these materials even improve properties, in
which case the word impurity leads to an erroneous conclusion concerning the
material. For example, certain phenolic, naphthenic acid, or sulfur-bearing
compounds are now being credited with giving jet fuel the lubricity needed by the
fuel pumps, and their removal from the fuel is being questioned.
In petroleum distillates, the non-hydrocarbon constituents ( impurities ) most
frequently present as sulfur, oxygen, and nitrogen derivatives of hydrocarbons.
There can be wide variation in the type of sulfur, oxygen, and nitrogen
compounds present and wide variation in their concentrations, depending among
other things upon:
Boiling range of the distillate - initial boiling point (IBP) to final boiling point
(FBP) - by the standard ASTM Distillation Method, ASTM D-86.
The source of the crude from which the distillate was produced.
Whether it is a virgin ( straight run ) or processed fraction ( cracked, reformed,
desulfurized or otherwise processed ).
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Whether or not the sample is fresh or has aged in the presence or atmospheric
oxygen.
It should be kept in mind that there may be compounds present that contain more
than one and in some cases all of these elements.
When metallic compounds are found in distillate products, it is reasonably certain
that they came from an extraneous source. For example, copper may get into a
fuel oil by a reaction of a naphthenic acid or mercaptan in the oil with copper in a
line or heat exchanger.

2.1.1. Pretreatment Section

2.1.1.1. Function

The caustic prewash by 3o Be caustic injection removes undesirable acidic

compounds in the kerosene such as naphthenic acids, H2S and CO2. Also, as long
as the prewash caustic contains some free sodium hydroxide, slightly weaker
acidic compounds such as light mercaptans will also accumulate in the caustic.
Caustic wash solution is generally effective until 50% spentness. Since fresh 3o Be
caustic is injected continuously, there should be no trouble anticipated.
Naphthenic acids are harmful in Merox treating by mechanically interfering with
the sweetening. Absorbed naphthenic acids plug the catalyst pores. Naphthenic
acids also react with metals particularly copper, to form gelatinous precipitates
which can cause plugging of screens, pump valves and meters and control valves.
Also, naphthenic acid or its metallic salt is surface active and stabilizes emulsion.
H2S and CO2 are undesirable because they react with and consume free sodium
hydroxide in the Merox reactor. If sodium sulfide is produced ( Na2S ) from H2S
neutralization, it will then consume the oxygen needed for mercaptan oxidation
and carbonates precipitate will plug screens and valves.
Caustic prewashing, properly operated, should yield no more than 0.15
mgKOH/gm acid number ( AN ) in the kerosene.

2.1.1.2. Mixing Valve Pressure Drop

The mixing valve provides intimate contact of caustic and kerosene. The higher
the mixing valve pressure drop, the better the contact and reaction between the
caustic and kerosene thus the outlet acid number is lower. Normal mixing valve
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pressure is set at least 0.70 kg/cm2 and can be increased to 1.5 kg/cm2 provided it
does not cause poor coalescing and high amperes in the electrostatic Coalescer.
The acid number measures the amount of organic acid ( mainly naphthenic acid )
in kerosene. Therefore low acid number of kerosene after the coalescer indicates
good organic acid removal. The acid number from electrostatic coalescer should be
controlled below 0.015 mgKOH/g.

2.1.1.3. Electrostatic Coalescer Temperature

Electrostatic coalescer temperature must be controlled below 50 oC. It is to

prevent caustic embrittlement to occur at high temperature.

2.1.1.4. Pre-wash Caustic

The 3o Be ( about 2% wt ) caustic used for pre-washing in the electrostatic

coalescer is important. It removes impurities like naphthenic acids and phenols to
prevent accumulations of naphthanates in catalyst which can greatly reduce
catalyst activity. Phenols, if not removed, can cause product coloration.
Normal recommended caustic soda strength is 1.0% to 3.0% weight. If the caustic
strength increases above 3% strength, sodium naphthanates become insoluble in
the aqueous phase and the carry over to the reactor will occur. It makes oil
discolored and the caustic will look like light tea color rather than dark brown
which is indicating decrease in sodium naphthanate solubility. Too low caustic
concentration will cause a thick creamy emulsion like salad dressing at the
interface. Oil will be hazy and will not settle into clear and bright easily. It also
turns those caustic in the reactor into a highly viscous and dark brown in color.
Naphthanates carry over will foul catalyst. This gives rise to a highly viscous
dark brown colored caustic from the reactor and must be drained away.
The 3o Baume caustic is injected from the 3o Be Caustic Storage Tank ( 801-TK2 )
to the inlet line of the mixing valve by Caustic Injection Pumps ( 801-P2A/B ).

2.1.2. Sweetening Section

2.1.2.1. Reaction Temperature

Proper mercaptan oxidation proceeds at a reaction temperature of 38 - 49 oC and

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in an alkali medium. Reactor temperature can easily be controlled by the alkali
medium which is provided by periodically saturating the reactor bed with 10o Be
caustic solution. High temperature and concentrated caustic solution are
undesirable as some side reactions will take place to a greater extent. Certain
phenols, if present, will oxidize to form colors.
Peroxidation of thiophenols and tertiary mercaptans will lead to gum formation.
In Merox process, a temperature of 60 oC and caustic concentration of 20o Be are
generally regarded as the upper limits. Above these conditions, caustic
embrittlement must be considered.
The design operating temperature in the reactor is between 38 oC to 49 oC. The
higher the temperature the faster is the rate of reaction and lowers the outlet
mercaptans. Too high a temperature may affect the product color due to increase
in side reactions.
Proper mercaptan oxidation proceeds at a reaction temperature of 38 oC - 49 oC in
an alkali medium.

2.1.2.2. Pressure

Pressure is not considered an operating variable. However, the pressure must be

sufficient to keep all the air used dissolved in the kerosene. Channeling will take
place through the reactor if a separate air phase is present. A design back
pressure of 5.27 kg/cm2G is considered sufficient.

2.1.2.3. Air

Oxygen for the oxidation of mercaptan comes from the air injected into kerosene
to the reactor.
The formula for calculating the theoretical air required for different kerosene feed
mercaptan concentration and throughput is given above ( Refer to Section 2.1 -
Process Variables ).
Normally, set the air flow to 1.5 to 2 times higher than theoretical air to ensure
good reaction.

2.1.2.4. Catalyst Activity

The performance of the Kerosene Merox unit is based on its ability to convert
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mercaptan into disulfide. The mercaptan content of the reactor outlet must be
checked at regular intervals or as and when required. The product specification of
Jet A-1 specified that the maximum mercaptan content is 10 wt ppm.
Doctor’s Test will show a “positive” when mercaptan content is more than 10 ppm,
so it is a convenient test method for plant control.
The chemical reaction of Doctor solution and mercaptan is as follows:

2 RSH + Na2PbO2  (RS) 2Pb + 2NaOH

(RS) 2Pb + S  R2S2 + PbS ( Black color )

When the product fails the Doctor’s Test or Mercaptan Sulfur’ specification, the
following actions must be taken :
 Check the air injection rate. Increasing air rate will usually help to lower the
mercaptan content.
 Check the air mixer to ensure it is not damaged.
 Raise the reaction temperature.
 Resaturate reactor bed with 10o Be caustic. The 10 o Be caustic is prepared by
diluting 25o Be caustic with condensate at 10o Be Caustic Storage Tank
( 801-TK1 ).
As the catalyst activity declines, there will be a need for more and more frequent
resaturation of the catalyst with caustic. Finally, at the time of imminent catalyst
change, even continuous caustic circulation will no longer give a product of
satisfactorily low mercaptan content.
As stated above, the solid catalyst absorbs certain high molecular weight trace
materials from the hydrocarbon. When the catalyst is resaturated with caustic,
some of this absorbed material will be washed off the catalyst. The caustic used
for resaturation of the catalyst acquire a brownish discoloration. Continued use of
this caustic for resaturation will lead to premature catalyst activity decline.
A single batch of caustic should not be used for more than about two to four
resaturation cycles depending upon the amount of material absorbed from the
stock treated.
There is no way to determine how many times it is safe to re-use the caustic,
except by its appearance based on personal judgment and experience.
From time to time if there appears to be a decline in catalyst activity, washing the
catalyst with hot water to remove the adsorbed materials that interfere with its
performance may give a partial restoration of its activity.
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Hot water wash the catalyst bed if pressure drop of the reactor exceeds 0.70
kg/cm2G or the reactor temperature is above 50 oC and air exceeds twice the
theoretical amount and Doctor Test remains positive. Condensate is heated in
Water Heater ( 801-ME5 ) by low pressure steam to about 93 oC. Washing the
catalyst with hot water may help to remove sundry organic compounds and
caustic neutralization soap which have deposited in the charcoal pores or
otherwise physically blocked off the active catalyst surface. Resaturate with
caustic after hot water wash. ( See Section 6.4 - Hot Water Wash for more
information ).
Reimpregnate the catalyst with Merox catalyst if hot water wash needs to be
carried out too frequently. Frequency is expected to be once a year. ( See Section
6.4 - Re-impregnation for more information ).

2.1.3. Post Treatment Section

To meet the stringent jet fuel specifications in thermal stability and water
tolerance, post treatments are provided by water wash, salt filter and clay filter.
Wash water removes the soluble surface active materials and the entrained
caustic in the kerosene and then saturated water in the kerosene stream will be
decreased in the salt filter. The clay filter absorbs the insoluble surface active
materials, metals and particulates. Used water in the water wash must be
replaced frequently, usually every day. Pressure across the salt filter must be
measured for the bed height. Pressure drop across clay filter must be less than 1.0
kg/cm2.
Corrosion
Hydrogen sulfide and active mercaptan in the kerosene if not removed in the
electrostatic coalescer will cause the kerosene product to fail the copper corrosion
test.
Thermal Stability and MSEP
High copper ion in the oil will affect the thermal stability and high naphthenic
salt and other surfactants will affect the MSEP. Naphthenic salt is removed by
water wash and copper ion and non-water soluble surfactants are removed by the
clay filter.
1. Fresh wash water when required is injected into the bottom of the Water
Wash ( 801-V3 ) by the Wash Water Pump ( 801-P5 ). The washed water is
withdrawn from the bottom of the drum when the total alkalinity exceeds
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approximately 0.2 wt% NaOH or a pH of about 12.5.
2. Check salt filter bed height at least once a month by measuring pressure drop
across the bed. Provide 66.8 m3 of commercial grade rock salt which will pass
through U.S. Sieve series no. 2-1/2 and is retained on a no. 6 sieve.
3. This is for the initial loading of the salt drier. Half this quantity will be
required for the refill. The estimated days on stream for the salt drier before
reloading, based on consuming half the salt, is approximately 240 days.
4. Pressure drop across the clay filter must be less than 1.5 kg/cm2. Back wash
the bed and/or fluffing the bed with nitrogen to reduce the bed pressure drop.
Bed skimming operation or replacement should be carried out if the
differential pressure across the bed is still high after back wash and N2
fluffing. In this case, the switch over from onstream clay filter ( 801-V5 ) to
the bypass line should take place.

2.2. Process Flow and Control

2.2.1. Description of Process Flow

Merox sweetening process, which is licensed by UOP Inc. Ltd., is adopted for this
unit. The unit consists of the following major sections: the Pre-treatment Section
for the removal of naphthenic acids, the Sweetening Section ( Merox proper) for
the removal of mercaptans, and the Post-treatment Section.

Pretreatment Section
The function of the pretreatment section is to remove naphthenic acids in the feed
kerosene. If naphthenic acids are not removed, sodium naphthenates are formed
in the sweetening reactor, which is surfactants, coat the catalyst and block the
pores of charcoal catalyst support.
Therefore, naphthenic acids must be reduced to a tolerable level prior to
sweetening. This is achieved by using an alkaline prewash. An electrostatic
prewash is used for this unit.
Sweetening Section
Mercaptans are directly converted to disulfides in a fixed bed reactor system. The
disulfides remains in the product. There is no reduction in total sulfur content.
Because the vapor pressure of disulfides are so low relative to those of
mercaptans, their presence is much less objective.
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The sweetening section consists of a reactor which contains a bed of specially
selected activated charcoal impregnated with Merox reagent and wetted with
caustic solution.
Air is injected in the feed kerosene ahead of the reactor and is passing through
the catalyst impregnated bed, the mercaptans in the feed are oxidized to
disulfides.
The reactor is followed by a settler which also serves as a caustic reservoir. A
caustic circulation pump is provided for intermittent circulation from the settler
to wet the catalyst bed. See figure 2.2.
Figure 2.2
Kerosene Fixed Bed Merox

Air
H2S Merox
Free Catalyst
Sweet
Reacto Produc

Causti
Merox
c
Plus
Legend: Caustic
---- = Intermittent Circulatio

Post-treatment Section
This section consists of a water wash to remove entrained caustic solution and
water soluble surfactants which may have been present in the sweetened
kerosene, a salt filter to remove any entrained or dissolved water and a clay filter
to remove any insoluble particles.

2.2.1.1. Pre-treatment Section

Raw kerosene from the CDU is routed directly to the Electrostatic Coalescer
Prewash ( 801-ME7 ) at a pressure of 8.4 kg/cm2G and at a temperature of 40 oC.
The feed kerosene, before it enters the 801-ME7, is mixed with 3o Be caustic
solution by means of an adjustable mixing device. The 3o Be caustic solution is
supplied by the Caustic Injection Pumps ( 801-P2A/B ) from the 3o Be Caustic
Storage Tank ( 801-TK2 ). Naphthenic acid in the kerosene stream is neutralized
by the caustic and the spent caustic settled in the 801-ME7 is discarded to the
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Effluent Treatment System under an interface level control.
When an excess of NaOH is available, the chemical reaction is :
RCOOH + NaOH  RCOONa + H2O

2.2.1.2. Sweetening Section

An air compressed by the Air Compressor System ( 801-C1A/B ) is mixed with the
kerosene discharged from 801-ME7.
A small stream ( 15.3 liters/hr maximum ) of catalyst activator ( Merox Plus ) is
injected into the kerosene stream after the addition of the air by the Merox Plus
Injection Pumps ( 801-P3A/B ).
The combined stream ( kerosene, catalyst activator, air ) passes through a bed of
Merox catalyst in the Reactor ( 801-R1 ) where the mercaptans are oxidized to
disulfides ( sweetening ).
The chemical reaction in the presence of the Merox catalyst and at an alkaline
condition is:
2RSH + ½ O2  RSSR + H2O

The reaction temperature varies from 38 to 49 oC depending on the feed

mercaptan, feed type and catalyst condition. The operating pressure is maintain
at a level to ensure injected oxygen soluble in the kerosene for reaction by a back
pressure controller installed at the kerosene rundown line.
The sweetened kerosene from the Reactor ( 801-R1 ) flows into the Caustic Settler
( 801-V1 ) for gravity separation of any entrained caustic.
10o Be caustic solution is prepared by diluting 25o Be caustic solution with
dilution water in the 10o Be Caustic Storage Tank ( 801-TK1 ) and used for
batchwise caustic re-saturation of the catalyst bed. This 10o Be caustic solution is
transferred from 801-TK1 to the Caustic Settler ( 801-V1 ) by Caustic Transfer
Pumps ( 801-P1A/B ). From 801-V1, the solution is circulated to the inlet line of
the Reactor ( 801-R1 ) by Circulation Pumps ( 801-P4A/B ). The circulating caustic
is settled in 801-V1 during the resaturation process of the catalyst bed.

2.2.1.3. Post Treatment Section

The treated kerosene from 801-V1 is fed into the Water Wash ( 801-V3 ) to remove
entrained caustic solution and water-soluble surfactants. The wash water, when
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required, is injected by the Wash Water pump ( 801-P5 ) at the bottom of the
801-V3. The waste water is withdrawn from the bottom of the 801-V3 to the
Effluent Treatment System. Water change-out is normally made when the total
alkalinity exceeds approximately 0.2 wt% NaOH or a pH of about 12.5.
The washed kerosene from 801-V3 is introduced into the Salt Filter ( 801-V4 ) and
then saturated water in the kerosene stream will be decreased therein. The brine
water from 801-V4 is withdrawn intermittently by manual operation.
The last essential step in the kerosene treating process is clay filtration, which
serves basically as a final clean-up step to assure a kerosene product that is free
of solids, color bodies, water and soaps.
The Salt Filter immediately ahead of the Clay Filter ( 801-V5 ) protects the clay
from being rendered ineffective prematurely by free water.
The treated kerosene product is run down to Tankage and Blending System at a
pressure of 3.52 Kg/cm2G and at a temperature of 40 under pressure control.

2.2.2. Control Flow Plan

2.2.2.1. Feedstock control flow scheme

Feed to this unit will be on flow control in the upstream unit. The location of the
feed flow control valve will be determined during the process design.
Refer to Figure 2.3.
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FI
CDU KMX
FIGURE 2.3 FEED 003A

TO 801-ME7

100-V9 FI
LY HSS 003B
LY
069 069

LIC LY
069 069 FIC
009

FUEL OIL
BLENDING

100-V1 100-EA1

Heat
Recovery
LIC
080

LY HSS FUEL OIL

069 BLENDING
100-E2A/B
FIC
213

HSS = HIGH SELECTOR

100-V1
801-P9A/B
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2.2.2.2. Product control flow scheme

Product from the Kerosene Merox Process Unit will be routed to the Kerosene
Storage through a pressure controller located downstream of the clay filter
( 801-V5 ).
Refer to Figure 2.4.

FIGURE 2.4 PRODUCT

CO O
801-V3 801-V4 801-V5
KMX OFFSITE

SR

TO
STORAG
E

FIR PIC
023 008 HSS
FY
174

FRC
192

JP-1
KEROSENE

SR = SPLIT RANGE HSS

FY
173
HSS = HIGH SELECTOR SWITCH
FRC
170

JP-4
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3. EMERGENCY EQUIPMENT

3.1. Safety valves

Summary of the safety valves provided for this unit is shown below:
Refer to “DATA SHEET FOR SAFETY RELIEF VALVES”
( S-801-1374-301 )

Tag No Set Press. Size and Service Location Governing

kg/cm2g Type Relief Case
801-PSV-001A/ 24.7 3/4*3/4 801-P2A/B Discharge Blocked Outlet
B
801-PSV-002A/ 22.8 2H3 801-R1 Top Fire
B mounted
801-PSV-003A/ 22.6 1.1/2G3 801-V1 Top Fire
B mounted
801-PSV-004A/ 22.8 1.1/2G3 801-V3 Top Fire
B mounted
801-PSV-005 36.1 3/4*3/4 801-P3 Discharge Blocked Outlet
801-PSV-006A/ 23.3 2H3 801-ME-7 Top Fire
B mounted
801-PSV-007A/ 22.9 1.1/2G3 801-V4 Top Fire
B mounted
801-PSV-008A/ 23.1 2H3 801-V5 Top Fire
B mounted

3.1.1. Summary of Flare Loads

Refer to “ FLARE LOAD SUMMARY”( S-801-1223-701)

3.2. Car sealed valves

Car Sealed Open or Car Sealed Close valves are listed below.
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Positio Line No. / Service Size Equipment / P&ID No.
Line No.
n

Open 801-PSV-006A inlet line 3” 801-3”-FL-1502 D-801-1225-11

-A2A1P
5
Open 801-PSV-006A discharge 3” 801-3”-FL-1501 D-801-1225-11
-A1A1
line 5
Close 801-PSV-006B inlet line 3” 801-3”-FL-1502 D-801-1225-11
-A2A1P
5
Open 801-PSV-006A discharge 3” 801-3”-FL-1501 D-801-1225-11
-A1A1
line 5
Open 801-ME3 2” 801-3/4”- D-801-1225-11
Removable Injection CH-1504-A2A1
5
Nozzle P
Open 801-PSV-002A inlet line 3” 801-3”-FL-1603 D-801-1225-11
-A2A1P
6
Open 801-PSV-002A discharge 3” 801-3”-FL-1601 D-801-1225-11
-A1A1
line 6
Close 801-PSV-002B inlet line 3” 801-3”-FL-1603 D-801-1225-11
-A2A1P
6
Open 801-PSV-002B discharge 3” 801-3”-FL-1601 D-801-1225-11
-A1A1
line 6
Open 801-PSV-003A inlet line 3” 801-3”-FL-1604 D-801-1225-11
-A2A1P
6
Open 801-PSV-003A discharge 3” 801-3”-FL-1602 D-801-1225-11
-A1A1
line 6
Close 801-PSV-003B inlet line 3” 801-3”-FL-1604 D-801-1225-11
-A2A1P
6
Open 801-PSV-003B discharge 3” 801-3”-FL-1602 D-801-1225-11
-A1A1
line 6
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Open 801-PSV-004A inlet line 3” 801-3”-FL-1702 D-801-1225-11
-A2A1P
7
Open 801-PSV-004A discharge 3” 801-3”-FL-1701 D-801-1225-11
-A1A1
line 7
Close 801-PSV-004B inlet line 3” 801-3”-FL-1702 D-801-1225-11
-A2A1P
7
Open 801-PSV-004B discharge 3” 801-3”-FL-1701 D-801-1225-11
-A1A1
line 7
Open 801-PSV-007A inlet line 3” 801-3”-FL-1803 D-801-1225-11
-A2A1P
8
Open 801-PSV-007A discharge 3” 801-3”-FL-1801 D-801-1225-11
-A1A1
line 8
Close 801-PSV-007B inlet line 3” 801-3”-FL-1803 D-801-1225-11
-A2A1P
8
Open 801-PSV-007B discharge 3” 801-3”-FL-1801 D-801-1225-11
-A1A1
line 8
Open 801-PSV-008A inlet line 3” 801-3”-FL-1804 D-801-1225-11
-A2A1
8
Open 801-PSV-008A discharge 3” 801-3”-FL-1802 D-801-1225-11
-A1A1
line 8
Close 801-PSV-008B inlet line 3” 801-3”-FL-1804 D-801-1225-11
-A2A1
8
Open 801-PSV-008B discharge 3” 801-3”-FL-1802 D-801-1225-11
-A1A1
line 8

3.3. Remote Operating Valves

Remote operating valves are not provided in this unit.

3.4. Instrument alarms

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Instrument alarm types are listed below. Set values of each alarm are also shown

(1) Level alarm

Unit: %
Tag Service AL AL AH AHH P&ID No.
No. L

LI-002 10o Be Caustic Storage 2.9 D-801-1225-113

Tank Level
LI-001 3o Be Caustic Storage Tank 10.5 D-801-1225-113
Level
LIC-30 Electrostatic Coalescer 20 80 D-801-1225-115
Prewash Interface Level
3

(2) Temperature Alarm

Unit: ℃
Tag No. Service AL AL AH AHH P&ID No.
L

TI-091 Air Compressor System 60 D-801-1225-114

discharge temperature

(3) Flow Alarm

Unit: m3/h(liquid) or Nm3/h(gas)
Tag No Service ALL AL AH AH P&ID No.
H
FI-003A/ Kerosene Feed to Mixing 50 65 D-801-1225-11
B valve 5
FIC-004 Compressed air to Air Mixer 17 D-801-1225-11
5
FI-023 Treated Kerosene to 65 D-801-1225-11
Tankage 8
FI-120 Cooling water Header 98 D-801-1225-13
3
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(4) Pressure Alarm

Unit: kg/cm2g
Tag No Service ALL AL AH AH P&ID No.
H

PI-011 Air Compressor System 8.5 D-801-1225-11

discharge pressure
4

(5) Differential Pressure Alarm

Unit: kg/cm2
Tag No Service ALL AL AH AH P&ID No.
H

PDI-017 801-R1 Reactor 0.9 D-801-1225-11

differential pressure
6
PDI-007 801-V5 Clay Filter 1.5 D-801-1225-11
differential pressure
8

(6) Other Alarm

Tag No. Service P&ID No.

XA-021A/B/E/F Seal system trouble for D-801-1225-112
801-P4A/B
XA-020A/B/E/F Seal system trouble for D-801-1225-113
801-P1A/B
XA-901B/F Seal system trouble for D-801-1225-113
801-P1A/B
XA-202A/B Common alarm for 801C1A/B D-801-1225-114

3.5. Instrument trip settings

Trip settings that cause the plant to shut down are listed below. Refer to “CAUSE
AND EFFECT CHART “ ( S-801-1371-401 ) on Attachment 9.12 for details.
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Tag No. Service Trip Set P&ID No.

FSLL-003A/ Raw Kerosene to Electrostatic 50 m3/h D-801-1225-115

B Coalescer Prewash
( 801-ME7 )

3.6. Procedures for setting protective relays

Access control to various manipulations on DCS for this project is shown below
and details of operating procedures is shown in the DCS vendor's operating
manual :
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Operator Superviso Engineer

r

Controller SP x x x
Alarm SP x x
PID Tuning Constants x
Other Parameters x
( e.g. dir/rev )

Access control to various manipulations on ESD PLC for this project is shown
below and details of operating procedures is shown in the DCS vendor's operating
manual:

Operator Supervisor Engineer

Trip SP x
Other Parameters ( e.g. x
Timer )
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4. PREPARING THE UNIT FOR PRE-COMMISSIONING

4.1 Pre-commissioning

As the construction of the unit nears completion, a large amount of work must
begin in order to prepare it for start-up. These pre-commissioning activities have
three main purposes:
 To ensure, by thorough inspection and testing, that the unit is safe,
operable, and constructed as specified;
 To operate equipment for by flushing, running in, etc. and
 To acquaint the operators with the unit.
The importance of these activities cannot be overemphasized. No matter how well
a unit is designed, if the equipment is not as specified, not properly brought on
stream. Or not understood by operators, it will not perform as expected.
All of the following activities are required to properly pre-commission this unit.
However, an exact order of presentation need not be strictly obeyed. Depending
on the progress of construction, certain procedures may be required earlier or
later that suggested here. A thorough knowledge of the entire pre-commissioning
operation will allow the plant personnel to schedule activities in the most
time-saving and labor efficient way. These are the necessary pre-commissioning
activities:
1. Vessel Inspection
2. Inspection of other Major Equipment
3. Piping and Instrument Check
4. Hydrostatic Testing
5. Line Flushing
6. Run-in of Pumps and Drivers
7. Servicing and Calibration of Instruments
8. Commissioning of Utilities
9. Availability Check of Chemicals, Catalysts, and Other Materials
10. Plant Pressure Test
11. Air Freeing
12. Commissioning of Additional Plant Services

4.1. Commissioning of Utilities

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Utilities are placed in service during commissioning ( preparation for start-up ).
However, it should be verified that all utilities are in service or in readiness prior
to start-up. Lines should be flushed and leak tested. Steam lines should be
warmed up slowly to prevent damage from water hammer. All steam traps and
control valves are to be placed into service and tested. The following list of
systems should be commissioned:
1. Plant water and treated water systems. These systems should already have
been commissioned prior to the line flushing procedure.
2. All electrical and light systems, including emergency power backups.
3. All plant and instrument air systems.
4. Nitrogen system.
5. Steam and condensate systems, excluding steam tracing for the moment.
6. Condensate systems, receiving condensate from steam traps of several steam
systems noted above, are ready for service. All steam traps should be checked
for operability.
7. All drains and effluent systems.
8. All fire fighting and other emergency equipment.
9. All storage tanks must be thoroughly flushed, leak tested, dried, and perhaps
air-freed if the tank is in hydrocarbon service. Those tanks that have been
air-freed should be left under slight positive nitrogen pressure. All lines to
and from tankage must be flushed, blown dry with nitrogen, and pressure
tested.
The steam tracing, plant cooling water, and flare systems will be commissioned
after the plant pressure test has been completed.

4.2. Pressure Testing

After all fabrication has been completed the unit vessels and piping should be
pressure tested hydraulically. Hydrostatic tests are made on new or repaired
equipment to prove the strength of materials and welds. This test is made by
completely filling the equipment with water ( typically ) and increasing the
pressure. Normally a positive displacement pump will be used to raise the
pressure. This test is normally performed by construction personnel and it should
not be confused with other less severe tests generally carried out before a start-up
to check the tightness of connections.
1. Vessels that have met hydrotesting requirements in the fabricators shop may
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be isolated from the hydrotest if desired and if allowed by applicable codes.
Before hydrotesting any vessel it should confirmed that the vessel is designed
and supported such that it can be safely be filled with water. If not, the
applicable code should be consulted for testing.
2. Care should be taken not to exceed the pressure rating of any vessels or
equipment when preparing a hydrotest circuit. Internals, such as displacers,
level ball floats, or other instruments not designed for the test pressure must
be removed. All relief valves ( PSV’s ) should be removed, blinded, or gagged
during the hydrotest. Since all relief valves must be bench tested and set
before final installation, it may be desirable to perform the testing at this
time.
3. Vents must be provided at all high points of vessels and piping in the
hydrotest circuit(s) to purge possible air pockets while filling.
4. All internal valves within a test circuit should be confirmed open.
5. Usually the hydrostatic pressure test is carried out at 1.5 times the design
pressure, but the proper test pressure must be confirmed for each vessel or
piping circuit in question.
6. Care should be taken that the temperature is not too low, causing the metal
to become brittle. The vessel/piping and water temperature should always be
above 15.5 oC to eliminate the possibility of cold-fracturing the metal.
Note that a water filled system requires venting when being drained in order to
avoid pulling a vacuum and possibly collapsing equipment.

4.3. Flushing out

All piping must be thoroughly clean of debris and scale. This may be done after
hydrostatic testing, before the test water is drained. Care must be taken not to
flush debris into equipment.
Generally, liquid lines are flushed with water and thoroughly drained. Water
flushed lines which do not drain freely should be blown clear with air. Gas lines
may be either water flushed or air blown, but water should be blown from gas
lines if water flushed. Gas lines to compressors must be free of water.
The following items are suggested as guide for line flushing:
1. Where practical, clean water should be supplied to the vessels, and
continuous lines should be flushed away from the vessel. Never flush into
equipment.
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2. No matter what the flushing medium - steam, air, or water - maximum
volume and velocity should be used for thorough cleaning.
3. Remove orifice plates before flushing.
4. Control valves and in-line instruments should be removed.
5. Instrument lines should be closed off or disconnected. The instrument air
header should be thoroughly blown with clean, dry air.
6. Relief valves should be blinded if they have been returned to service following
hydrostatic test.
7. Regulate the flushing medium at its source. As examples, water from a vessel
should be regulated at the vessel; and steam, at the valve in the supply to the
line being blown.
8. Where possible, flush downward or horizontally.
9. Always flush through a piece of equipment’s bypass to an open end before
flushing through the equipment.
10. Disconnect lines and exchangers and flush to the openings.
11. Flush through all vents and drains.
12. At pumps:
 Disconnect suction and discharge piping and flush lines. Do not
introduce any fluid into pump casing before cleaning the pump suction.
 Install temporary screens in pump suction strainers.
 Reconnect lines for circulating water.
 See further discussion under “Run-in of Pumps and Drivers”.
13. Flush or blow:
 The main header, from source to end, then
 Each lateral header, from the main to end, and
 Each branch line, from the lateral header to end.
14. For steam systems, flush well through dirt leg drains and steam trap
bypasses before placing the traps in service.
15. Supply steam lines to ejectors should be disconnected while being cleaned.
16. Flush through open end lines. Do not restrict flow in principle.
17. After placing the steam traps in service, check whether the traps operate
properly.
18. After flushing operation, check that all orifice plates are installed and
positioned correctly as per list.
19. When necessary vessels or drums are used as water reservoirs for flushing,
check vessels for water-filled design. Moreover, a water-filled system must
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not be drained without adequate venting to avoid a vacuum condition and
probable collapse of equipment not designed for vacuum.
Upon completion of line flushing of any system, carefully check that all temporary
breaks are reconnected, control valves are replaced, and pumps alignments are
normal. Also, verify that all free water has been drained.

4.4. Acid Cleaning of Reciprocating Compressor lines

Not applicable to this unit.

4.5. Inspection and Run-in of Pumps and Fans

Proper installation and operation of pumps and drivers is essential for

trouble-free performance. The pumps and drivers should receive careful handling
during initial run-in. The initial run-in of pumps is generally done by circulating
water through the new equipment. Temporary strainers are installed in the
suction line of the pumps, conveniently located for removal and cleaning. The
screens should be positioned so that dirt particles will not gravitate to
inaccessible places when flow is stopped. During run-in of pumps, the strainers
may cause some restriction of flow. As debris collects in the strainers, flow to the
pumps will fall off. When this happens to a centrifugal pump, it will be necessary
to throttle the pump discharge by partially closing the discharge valve. This will
prevent the pump from cavitating, which can cause damage to the pump.
However, also avoid restricting the pump discharge to the extent that it causes
internal slippage and excessive heat generation.
In starting a turbine driven centrifugal pump, the rotation should be brought up
to the speed as rapidly as possible. Normal operating speeds are usually attained
rapidly and automatically with motor-driven pumps, assuming proper motor
starting.
The development of discharge pressure is essential to flush and lubricate the
wearing rings. After initially starting the pump, close the discharge valve for a
short time.
Subsequently, it is always advisable, where practical, to close the pump discharge
valve immediately prior to shutting down a centrifugal pump. However,
discharge valves on operating positive displacement pumps should never be
closed. These pumps can over pressure themselves and downstream lines and
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equipment. The following items are suggested for checking prior to run-in:
1. The manufacturer’s operating instructions for any specific precautions that
should be observed.
2. Completion of overall installation.
3. Alignment of pump and driver for cold operation. No undue strain by the
piping on the pump or driver is allowable.
4. Cooling fluid piping and seal or gland oil piping:
 Conventionally packed pumps in hot service are generally furnished with
gland oil. Verify that this installation is correct and complete.
 For pumps with mechanical seals, verify that all of the components of the
flushing system ( such as strainers, separators, restriction orifices, and
coolers ) have been correctly installed and are clean. Loss of flush or dirty
flush may cause the failure of seals.
5. Packing or seals are installed.
6. Bearings and shafts have been cleaned prior to final lubrication.
7. Pump and driver are lubricated according to lubrication instructions.
8. Rotation of electric motor drivers uncoupled from the pump. Run-in
uncoupled for a minimum of four hours, verifying good motor operation.
During run-in, many pumps are delivering a higher density liquid ( water ) than
the normal process fluid. But the pumps drivers are sized for the normal pumping
fluid. Consequently, there is potential for the overload of many electric motors. To
avoid overloading the motor of a centrifugal pump, the flow must be limited by
throttling the pump discharge valve. When doing so, if possible, check the
amperage usage against design.
The following procedure is suggested for pump run-in:
1. Rotate pump and driver by hand, verifying that they roll freely.
2. Check that run-in water circulation is lined up.
3. Open suction valves fully, venting air from piping and pumps, completely
filling with liquid.
4. Establish flow of cooling fluid, where required.
5. Check that lubrication is satisfactory.
6. Make sure that electric power is available from the switch gear to the starter
of the electric motor driver.
7. Barely open the discharge valve on the centrifugal pump.
8. Start the pump; if the pressure does not build immediately, stop and resolve
the problem.
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9. When the discharge pressure has increased satisfactorily after starting,
gradually open the discharge valve to obtain the desired flow rate.
10. In the event of unusual noise, vibration, overheating, or other abnormal
conditions, shut the pump down immediately. Correct the cause before
resuming use of the pump. Continue to check for abnormal conditions as
these may occur after prolonged operation.
11. Check shaft sealing; mechanical seals should show no leakage.
Conventionally packed stuffing boxes must always be permitted to leak
slightly to provide some lubrication and to prevent overheating. Stuffing box
gland nuts are generally only finger tight. A leaking mechanical seal will
show some leakage on start-up. However, after the pump is started and
stopped a few times, the leakage may stop.
12. Operate the pump, directing flows through all suction and discharge piping
circuits.
13. Inspect and clean screens as required.
14. Recheck and realign if required, after any disturbance of piping, such as
required for suction screen inspection if pipe flanges have to be parted for
screen removal.
15. When shutting down, close the discharge valve first, maintaining discharge
pressure while the pump rolls to a stop. This will protect against the pump
rolling backwards should the discharge check valve leaks, and gives the
wearing rings a quick flush.
After all lines available to a pump have had suitable flushing, the temporary
screen may be removed, but only after it has shown free of debris on two
successive examinations. The permanent strainers may then be installed where
required.

4.6. Leak Test

The purpose of the leak test is to check the piping and equipment for tightness of
flanges, connections, and fittings. These tests should not be confused with the
hydrostatic tests made during construction. Generally plant air or nitrogen is
used for this test.
Prior to test, all the instruments which have been unmounted in the previous
steps must be remounted.
The temporary isolating blinds must be removed for a final pressure test, but the
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battery limit blinds must remain in the closed position.
The tightness test must be conducted within certain blocks divided according to
the design pressure of each vessel.
 The recommended pressure for the tightness test is about 7.0 kg/cm2G
( available pressure in air system ) or the normal operating pressure,
whichever is smaller.
 Leakage shall be checked with soap solution.
 All flanges shall be checked for leakage and re-tightened, if leakage is found.
 During the tightness test, the operating pressure shall be maintained as
shown above.
 A final leak/pressure test with process fluids at working pressure is made as
part of the plant start-up described in the next section.
The test pressure should be held for a minimum of one hour, while every flange
and joint in the system is closely examined for leaks. Stubborn flange leaks may
often be stopped by simply unbolting and rebolting the flanges. Screwed
connections may require Teflon tape.

4.7. Inspection and Run-in of Reciprocating Compressor

Refer to the vendor’s operating manual of the Air Compressor System

(801-C1A/B).

4.8. Inspection and Run-in of Centrifugal Compressor

Not applicable to this unit.

4.9. Loading internal material required for absorbers, vessels, packed columns, etc.

4.9.1. Preparation of 10o Be and 3o Be caustic solutions

The Kerosene Merox Process Unit requires 3o Be caustic solution for neutralizing
naphthenic acids and 10o Be caustic for mercaptan oxidation reaction. The caustic
storage tanks ( 801-TK1 and 801-TK2 ) will be included for diluting the available
caustic to the required concentration. The caustic strength that will be used for
blending is 25o Be caustic.
10o Be caustic solution is prepared in 801-TK1 by diluting 25o Be caustic solution
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with cold condensate. This is done by filling first the tank with cold condensate to
a certain level then added with the required amount of concentrated caustic to
make the desired concentration. The tank is provided with plant air ( PA )
connection for mixing purposes to obtain a good mix of solution.
3o Be caustic solution is prepared in 801-TK2 by diluting 10o Be caustic solution
from 801-TK1 with cold condensate. 10o Be caustic from 801-TK1 is transferred to
801-TK2 by Caustic Transfer Pumps ( 801-P1A/B ). Prior to the transfer of the 10o
Be caustic to 801-TK2, the tank is filled first with cold condensate to the level
needed to have the desired concentration of the solution. 801-TK2 is also provided
with plant air connection for mixing.

4.10. Drying out Fired heater

Not applicable to this unit.

4.11. Drying out Reactor section

Not applicable to this unit.

4.12. Preparing Reactors

Refer to Section 6.4.1.4.( Catalyst Loading).

4.13. Loading Catalyst

Refer to Section 6.4.1.4.( Catalyst Loading).

4.14. Chemical boil-out of steam generation facilities

Not applicable to this unit.

4.15. Purging and gas blanketing

Before admitting hydrocarbons into any process lines or vessels, safe refinery
practice requires that the unit be freed of air. The air may be displaced with
water, steam, or inert gas, such as nitrogen. The system must be purged to
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prevent formation of explosive mixed gas prior to admitting flammable materials.
If steam is used, precautions should be taken to avoid the following potential
problems or hazards:
1. Collapse due to Vacuum: Some of the vessels may not be designed for
vacuum. This equipment must not be allowed to stand blocked in with steam
since the condensation of the steam will develop a vacuum. Thus, the vessel
must be vented during steaming and then immediately followed up with an
inert fuel gas or nitrogen purge at the conclusion of the steam-out.
2. Flange and Gaskets Leaks: Thermal expansion and stress during warm-up
of equipment along with dirty flange faces can cause small leaks at flanges
and gasketed joints. These must be corrected at this time.
3. Water Hammering: Care must be taken to prevent “water hammering”
when steam purging the unit. Severe equipment damage can result from
water hammering.
4. The following steps briefly outline air freeing by steam purging:
a. Portions to be steam purged include all the columns, vessels, heat
exchangers, and lines.
b. Pumps, sight glasses, level gauges and instruments are not to be
steamed-out. This can be done by closing their inlet and outlet valves. The
Electrostatic Coalescer is purged with the desuperheater immediately
before introduction of Feed oil.
c. When the unit is divided into a number of sections for steam purging, it
must be so arranged that steam is injected from one end of the section and
blown out from the other end.
d. Open high point vents and low point drains on the vessels to be steam
purged. After opening all vents and drains, steam purge is conducted by
opening the valve at the steam outlet and blowing in steam from the steam
out connection. Care must be taken not to cause hammering when
introducing steam. It may be necessary to make up additional steam
connections to properly purge some piping which may be “dead-ended”.
e. Thoroughly purge all equipment and associated piping of air. The progress
of the steam purge can be followed by marking up the P&I diagram to
indicate the lines purged. Verify that sufficient drains are open to drain the
condensate which will collect in low spots in the unit.
f. When the steam purging is completed, start to close all the vents and
drains. To prevent the creation of negative pressure within the system, the
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injection of a little steam must be continued until the subsequent filling of
fuel gas or nitrogen is started.
g. After steam purging all the sections of the unit, open all the block valves
that has been closed during the steam purging operation to enable the
subsequent fuel gas or nitrogen filling throughout the system.
h. Start to introduce fuel gas or nitrogen into all vessels and then cut back the
steam flow until it is stopped. Regulate the fuel gas or nitrogen flow and
the reduction of steam so that vacuum due to condensing steam is not
created in any vessel or that the refinery fuel gas system pressure is not
appreciably reduced. Introduce fuel gas or nitrogen into the system to
prevent vacuum. Maintain the pressure within the system at 0.5 ~ 1.0
kg/cm2G. When the system is under fuel gas pressure, check the O2 content.
( O2 content shall be less than 1.0 vol%. ). At every purging step, the
pressure of each equipment must be kept under its respective design
pressure.
i. For the steam purging operation of the Electrostatic Coalescer, special care
should be taken over the temperature of the steam ( Note ), or other
purging procedure selected, when the purge steam temperature is higher
than the design temperature.
Note: Steam-out temperature is limited to 120 oC for 801-ME7.
Desuperheater ( 801-ME6 ) is provided in order to reduce the steam temperature.

4.16. Pre-commissioning check list

This procedure describes in general terms the steps to be followed for placing the
unit on stream. The exact sequence of events depends on the flow scheme of the
particular unit. However, the following steps must be completed before charging
oil to the Unit.
1. All unnecessary blinds are removed,
2. All relief valves are tested and installed.
3. The flare header is purged and in service.
4. The sewers are in service.
5. All instruments and control systems are ready for service.
6. All utilities are in service.
7. All drains and vents are closed in the reactor section.
8. Control valves and bypasses are blocked in.
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9. All compressors are blocked in.
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5. COMMISSIONING

5.1. General overall commissioning plan.

Commissioning requires that many of the activities described in Section 4

Preparing Unit for Pre-commissioning have been completed and the feed oil can
be admitted into the unit.
The followings are a check list for RFSU ( ready for start-up ).
1. All equipment including instruments, etc. are ready for use.
2. All utilities are available for all the equipment.
3. Fresh caustic ( 3o Be and 10o Be ) have been prepared and stored in the 3o Be
and 10o Be Caustic Storage Tanks (801-TK2 and TK1) respectively.
4. Ensure all feeds, products, chemicals and effluents are properly lined up and
are ready to supply and receive materials.
5. All blinds or spectacle blinds have been placed in their respective operating
positions.
6. The portions, where the flammable materials are admitted, have been purged
and kept at positive pressure with fuel gas or nitrogen.
7. The line up for start-up has been completed. Insert the temporary mesh
strainers for start-up in the suction of pumps.
Refinery management and other sections concerned have been informed of the
proposed time of start-up.

5.2. Detailed step-by-step procedure

After the catalyst impregnation operation has been completed, the Kerosene
Merox unit is ready to be placed on-stream. The procedure for impregnation of
Merox FB reagent on the activated charcoal is described in Section 6.4.1( Special
Procedures ) of this manual.

5.2.1. Preparation for start-up

Remove all blinds from the unit as per blind list and confirm that all Merox unit
rundown B.L. blocked valves are blocked in.
Ensure that all RV’s and the flare system are purged and commissioned to the
main header.
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5.2.2. Nitrogen Pressure Up / Tightness Test

Ensure that all block valves from the Merox unit to rundown battery limit are
blocked off.
Fill the Water Wash ( 801-V3 ) and Electrostatic Coalescer ( 801-ME7 ) with
water up to the operating level and conduct nitrogen leaking test. Purge the
whole system then pressure up with nitrogen up to 3 kg/cm2G. Block in the
vessels and check flanges and manholes for leaks thoroughly with soap solution.

5.2.3. Unit Line up

The state of the unit at this time is as follows:

1. Catalyst in the Reactor ( 801-R1 ) has been saturated with 10o Be caustic.
2. Condensate has been pumped into the Water Wash ( 801-V3 ) up to the
operating level of half full.
3. Kerosene feed line from CDU is isolated at the unit B.L..
4. Mixing valve opened at 50%.
5. Electrostatic Coalescer Prewash ( 801-ME7 ) inlet and outlet valves are
opened. It’s bypass valve is shut and spent caustic line from 801-ME7 is
isolated.
6. Air injection valve ( FV-004 ) is shut.
7. Inlet valve of the Air Mixer ( 801-ME2 ) on the air line is opened.
8. Inlet and outlet valves of the Reactor ( 810-R1 ) are opened. All other lines
connected to the reactor are shut.
9. Inlet valve of the Water Wash ( 801-V3 ) is opened.
10. Inlet and outlet valves of the Salt Filter ( 801-V4 ) are closed and the valve of
the bypass line is open.
11. Inlet and outlet valves of the Clay Filter ( 801-V5 ) are closed and the valve of
the bypass line is open.
12. PV-008 downstream of the 810-V5 is closed.
13. 10o Be caustic has been already provided to a level of 25 % in the Caustic
Settler ( 801-V1 ), and also Merox Plus is ready for injection to the kerosene
feed line.
14. The treated kerosene line is lined up to the light slop header.
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5.2.4. Introduction of Feed

The unit is now ready to bring in feed from the Crude Distillation Unit ( CDU )
which is assumed to be sending the raw kerosene feed to the blending header.
1. Open the B.L. valve of the kerosene feed line and inform the CDU operators
that this unit is ready to receive raw kerosene.
2. Next step is ensuring that all the equipment in the unit is filled completely
with kerosene. This can be done by opening their respective PSV bypass lines
and observing the kerosene flow through the sight glass ( SG ) .
3. Commission the system pressure controller PIC-008 to raise the system
pressure up to 5.27 kg/cm2G.
4. Gradually increase the feed rate to its normal operating flow rate. Start
Caustic Injection Pump ( 801-P2A/B ) and Merox Injection Pump
( 801-P3A/B ) and inject into the kerosene feed. Initially, adjust the injection
rate of the 3o Be caustic based on feed acid no. of 0.02 mg/g.
5. Adjust mixing valve to give a pressure drop of about 0.7 kg/cm2G.
6. Turn on the power to 801-ME7 after ensuring that no more air is present.
7. Check interface at try cocks and commission LV-303 and send spent caustic
to 930-TK5 located at the Effluent Treatment System.
8. Control the reactor pressure at about 6.9 kg/cm2G and commission air
through FV-004 and air mixer to the reactor. Adjust air injection rate based
on feed mercaptan of 190 ppm as initial estimate and reaction temperature of
38 oC.
9. If the product is to be used for as jet fuel, commission the Salt Filter ( 801-V4 )
and Clay Filter ( 801-V5 ), after confirming that water carry-over is
minimized by visual examination of the product.
10. Check kerosene product for doctor test and adjust accordingly. Sample for
mercaptan sulfur content and flash point and send kerosene to storage tank
when it is on specification.

5.2.5. Final Plant Adjustment

The following items should be checked and, if necessary adjusted.

1. Air injection rate should be adjusted in conjunction with kerosene feed rate
and mercaptan sulfur loading.
2. Back pressure should be adjusted to ensure total air solubility in the system.
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3. Kerosene feed from the CDU unit should be kept at 38-40 oC initially, and the
treated product temperature should be kept at 40 oC rundown temperature to
storage.
4. 3o Be caustic injection rate should be adjusted, if necessary, to give an acid
number below 0.015 mgKOH/g in the kerosene feed to the reactor.
5. Follow the analytical plan in section 11.7.
Remember any changes made will not be detected immediately. Residence time in
the unit is 3.5-5 hours.

5.3. Special Precautions

1. Never activate the power to the Electrostatic Coalescer Prewash ( 801-ME7 )

and do not start the 3o Be caustic injection until 801-ME7 is liquid full of
kerosene ( LAL-302 disappears ).
2. When steam purging the system, the following precautions should be made
during operation.
Note: Although all equipment and piping is designed with steam-out
condition, care must be taken to prevent the potential problem and/or
hazards described below:
 Collapse due to vacuum by condensation of steam.
 Flange and gasket leaks due to thermal expansion and stress during
warming up.
 Water hammering.
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6. NORMAL START-UP AND SHUTDOWN

6.1. Normal Start-up after prolonged shutdown

The procedure used for starting up the Kerosene Merox unit after prolonged
shutdown is identical to the procedure used for initial start-up. ( See Section 5.2 -
Detailed Step by Step Start-up Procedure ).

6.2. Normal Start-up after short shutdown

After a shutdown of short duration, usually within 48 hours, and when kerosene
is still present in the unit, the unit can be re-started directly by feed introduction.
Follow the steps after filling up the equipment with kerosene in the start-up
procedure given in Section 5.2.

6.3. Normal Operations

6.3.1. Adjustment of Operating Parameters

The main operating parameters under direct control in the Kerosene Merox Unit
are the following:

6.3.1.1. Air Injection. Rate

The formula for calculating the amount of air necessary to convert all the
mercaptans to disulfides can be found in Section 2.1 ( Process Variables ). Using
this equation Figure 6.1 shows the required air injection rate as a function of feed
rate, specific gravity and mercaptan content for 1.5 times stoichiometric air.
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Figure 6.1
Air Injection Rate

( m3/hr
2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38
200

150
Basis: 30 scf of Air per
Mercaptan Sulfur
pound
in Feed, ( wt of Mercaptan
) 100
Example: If charge Rate is 32 m3/hr
and Mercaptan Sulfur is 104 wt
ppm

50 Then the Air Injection Rate

Should be 4 25 m3/hr

1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0
Air Injection Rate,

This plot is very useful in maintaining the correct air addition rate as the feed
properties fluctuate.
The amount of excess air should be minimized, however. Formation of a separate
air phase at the top of the Reactor, 801-R1 ( due to excessive air injection ) can
cause channeling to develop in the charcoal bed. An air phase collecting in the
reactor will gradually displace more and more hydrocarbon from the bed,
promoting channeling. This channeling continues even when the air phase is
subsequently eliminated. Sufficient pressure must be maintained in the reactor
to completely dissolve all of the air injected into the hydrocarbon.
Channeling essentially reduces residence time resulting in decreased mercaptan
conversion. Therefore, as a part of routine operation, the reactor overhead vent
line should be checked frequently for evidence of a separate air phase. If air is
found, it should be vented. The reactor pressure should be increased or the air
injection rate should be decreased in order to alleviate the problem.
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Another potential problem with excess air is the effect on kerosene color. If color
specifications are considered critical, then the amount of air injected should be
maintained between 1.10 and 1.25 times the theoretical amount. Otherwise,
depending on the crude source, the color could fall outside the specifications.

6.3.1.2. Caustic Circulation

By circulating on a regular basis, the basic environment required for the

sweetening reaction will be provided and the active catalyst will be cleansed.
UOP recommends to initially circulate twice per week for one hour at a rate of
10-20% of the hydrocarbon flow. The number of circulation will need to be
increased as the run time increases.
The caustic used for resaturation will acquire a brownish discoloration. A single
batch of caustic should not be used for more than about six resaturation cycles
depending upon the amount of material absorbed from the stock treated. As a rule
of thumb, if the caustic is a black color or if the caustic is more than 50% spent, it
should be changed out.

6.3.1.3. Pretreatment

Pretreatment in the Kerosene Merox is conducted to remove naphthenic acids. To

remove the naphthenic acids a dilute ( 2-3 wt% ) caustic solution is used to
neutralize the naphthenic acids to sodium naphthanate salts.
UOP has found that if the caustic strength is kept low ( 2-3 wt% ) and if the
caustic injection rate is maintained at the proper rate to spend the caustic no
more than 30%, the sodium naphthenates will exit with the water/caustic phase.
However, if the caustic strength is too high or the rate is too low, the sodium
naphthenates will form an emulsion with the hydrocarbon. The emulsion will
allow soaps to be laid down on the catalyst bed, causing a loss of activity. If the
problem is not rectified, the emulsion will coat the salt and allow water to pass
through the salt filter to the clay. In the worst case, the clay will become
saturated with water and will require replacement. Proper monitoring of the
pretreatment section is critical for successful unit operation.

6.3.1.4. Post Treatment

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Post treatment depends on mode of operation. If the unit is being run for
Kerosene production only, UOP would typically recommend bypassing the salt
filter and clay filter. The wash water is sufficient to remove any residual caustic
that might be carried over with the hydrocarbon. If the unit is being run for Jet
fuel production, then the salt filter and clay filter will need to be brought on
stream.

6.3.2. Operating Guidelines

Refer to the following table.

TABLE 6.1
Kerosene Merox Operating Guidelines

Prewash Caustic :
Gravity* 3.0 Be @ 15.5 oC ( max )
Total Alkalinity 1.7 - 2.0 wt%
Injection Rate

Kerosene After Electrostatic Coalescer/ Before Reactor :

Acid No. 0.01 mg KOH/g

Treated Product ( Kerosene / Jet Fuel ) :

MSEP / WSIM 90 min.
Separation Rating 2 max.
Interface Rating 1b max
RSH 10 wppm

Reactor Caustic :
Gravity 8 - 10 oBe
Total Alkalinity 5 -7 wt%
Consumption 28 - 56 kg NaOH per
1000 m3
Circulation Two times per week

Water from Water Wash :

pH 12.5 max.
Total Alkalinity 0.20 wt% max.

Kerosene Feed temperature 38 - 50 oC ( 55 oC max. )

Air Injection Rate See Air Injection Curves

6.3.3. Catalyst Deactivation

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Surfactant accumulation on the fixed bed catalyst results in gradual deactivation.
The surfactants can be additives used in crude oil production, recovery, and even
in processing. An example of the latter is certain corrosion inhibitors used in
fractionation columns.
When catalyst deactivation is so severe as to require reduced feed rate ( none of
the other control parameters will return the unit to satisfactory operation ),
reactivation is required. The reactivation procedure is given in Section 6.4.
Adjustment of the reactor temperature or use of a catalyst activity promoter can
extent the catalyst life before a reactivation of the catalyst bed is required.

6.3.3.1. Temperature

The sweetening reaction proceeds at normal run down temperatures, 38-50 oC .

As discussed earlier, the Kerosene Merox unit is normally operated at the lowest
temperature that will provide sweetening with a reasonable amount of excess air
( 1.25 to 1.50 times theoretical ). However, as catalyst bed deactivation occurs, it
is possible to raise the normal feed temperature in increments of 3 oC to offset
lost activity until time permits a shutdown and reactivation of the catalyst bed.

6.3.3.2. Merox Plus Additive Injection

Merox Plus is a catalyst activity promoter and can be used to extend the operating
life of the Kerosene Merox Unit. The solution is injected directly from the drum to
the feed stream using a small metering pump. Typical dosage rates are 50 to 100
wppm. The injection procedure is simple and can be found in Section 6.4 ( Special
Procedures ).

6.3.3.3. Feed and Product Stream Specifications

Tables 1.1, 1.2, and 1.3 list the hydrocarbon product specifications. The analytical
schedule, injection caustic specifications, and other operating guidelines for the
Kerosene Merox unit are shown in Table 11.1. These represent a minimum
recommendation for an adequate quality control program. Discussion of the
analytical methods is included in Section 11.7 ( Analytical Plan ) of this manual.
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6.4. Routine Operations

6.4.1. Special Procedures

6.4.1.1. Air Mixer Cleaning Procedure

Taken from Pall Process Filtration Corporation Bulletin

PSS 700C, p. 4
PSS Type 316L Element
1. Remove the filter element from the housing and remove the gaskets from the
filter element.
2. Remove excess process fluid. Degrease if oil contaminated.
3. Immerse the element slowly in a solution of 17% by weight sodium hydroxide
(chlorine free), 3% by weight sodium carbonate and 80% water. Boil for one
hour.
( Do not flow through element as caustic particles may be removed from the
cleansing fluid and clog filter medium. )
Caution : Safety controls for hazardous solutions are necessary. Bath
container must be able to safely accommodate hot caustic solution. Protective
clothing, hand, eye and face equipment required.
4. Rinse element with water to remove alkali.
5. Soak element in hot ( 93 oC) 14% nitric acid for 10 minutes. Nitric acid, 14%,
is made by adding 1 part of concentrated acid to 4 parts water.
6. Water wash in cold running water. Use Pall Ultipor, GF UIOOZ disposable
cartridge filters to prefilter the wash-water.
( If Pall filters are not used on the rinse water, do not force water through
filter as fine particulate matter in water will partially clog the porous
medium ).
7. Air dry at a temperature not to exceed 110 oC.
8. Install new gaskets on the element and return to service.
9. It is very important that none of these solutions is forced through the
element.

6.4.1.2. Hot Water Washing ( Figure 6.2 )

As operating bed life accumulates, realkalinization will become less and less
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effective in restoring Merox catalyst conversion activity. More frequent caustic
recirculation will become necessary. Finally even realkalinization with fresh
caustic will no longer sufficiently restore bed activity. At this point, the unit
should be shut down to allow a hot water wash of the charcoal bed.
Hot water washing is effective in removing the impurities that collect in the
charcoal pores. These materials are commonly salts such as sodium
naphthenates. The phenomenon of pore plugging and catalyst coating is gradual
and will generally allow the need for future hot water washing to be anticipated
and thus scheduled a convenient time.
Hot water wash facilities are provided in the unit. These facilities consist of the
Water Heater ( 801-ME5 ) and the Desuperheater ( 801-ME6 ).
Figure 6.2 Reactor Hot Water
Cold condensate is introduced to the Water Heater(801-ME5) and then heated by
low pressure steam therein. Vent Line
For the hot water washing procedure it is important to use a high-quality “soft”
water. Clean steam condensate or boiler feed water before any chemical additive
95-100
injection
oC
is normally acceptable.
Wash water should contain a low concentration of bicarbonates of calcium,
magnesium, and iron, etc. otherwise, the insoluble carbonates formed via the well
known “ water softening” reaction will deposit in the charcoal pores resulting in
reduced catalyst/charcoal life.
Steam
Ca(HCO3)2 + 2NaOH  CaCO3 + Na2CO3 + 2H2O
Nitrogen
The water used should have a total hardness of not more than 40 ppm as calcium
Connection
carbonate. Water

Sewer
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No free chlorine can be tolerated. Any chlorine present will attack and decompose
Merox catalyst reagent. For this reason city water supplies cannot normally be
used, even if very soft.
The following general procedure should be followed for hot water washing the
charcoal bed.
1. Stop air injection and route the hydrocarbon flow to off specification storage,
isolating the Reactor ( 801-R1 ).
2. Hydrocarbon should be drained, pumped out, or pressured out under steam
pressure or nitrogen.
3. Fill the reactor with warm, 50 oC wash water. Discard the wash water to
spent caustic facilities. Repeat. This step will greatly reduce the alkalinity of
the wash water discharged to the sewer system and will also protect the
vessel from caustic attack.
4. After the reactor has been drained and the major portion of residual caustic
has been removed, begin steam injection downflow at 60-100 kg/hr per cubic
meter charcoal. Steaming should continue until a small steam plum appears
at the reactor drain.
Caution: In no event should the steam temperature be permitted to exceed
190 oC , since the entry of air into the reactor may result in a fire due to
auto-ignition of the charcoal.
The purpose of this step is to remove most of the remaining hydrocarbons
from the charcoal and to heat the bed up prior to introducing hot water. For
high aromatic feedstock, the reactor drain effluent is usually cooled for safety
using direct cold water quench.
5. Commission the Water Heater(801-ME5) and introduce hot water at a
temperature of 95-99 oC via the reactor inlet distributor to fill the reactor
with hot water.
6. When the reactor is liquid full, begin draining the water effluent from the
drain at a rate equal to the hot water injection at 0.6 m3/hr per cubic meter
charcoal . The simplest method to ensure that the reactor remains full is to
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adjust the drain rate to keep a small flow out the overhead vent line.
7. During the initial stages of hot water washing, the reactor effluent from the
drain line will be highly discolored ( red, black or dark brown ), and foamy.
As the washing proceeds the water will lighten in shade and pass through a
series of color hues. Eventually the water will become clear and essentially
colorless.
8. At this point the water wash is essentially complete. However, if following
the water wash it is intended to continue with catalyst impregnation, the
washing procedure is considered complete when the effluent water pH has
been reduced to between 8 and 9. ( in that case, proceed to the neutralization
procedure ).
9. Gradually stop the steam flow, but continue to introduce cool condensate
through the water heater into the reactor to cold the charcoal bed down to a
temperature of about 60 oC. Nitrogen can be used to maintain the reactor
under a slight positive pressure. After the bed is cooled, the water is displaced
with nitrogen pressure and all of the water in the reactor is drained.
The unit can now be alkalinized and placed on stream.

6.4.1.3. Merox Plus Addition

Merox Plus is an activity promoter used for improving product quality, extending
catalyst life and reducing air and caustic consumption. Merox Plus is supplied in
1250 liter drums as part of a cycle drum system. The use of cycle drums
eliminates the concern of disposing non-returnable drums. The solution is
injected directly from the drum to the feed stream using the Merox Injection
Pumps ( 801-P4A/B ).
Begin injection of the Merox Plus solution at a rate of 50 - 100 wt-ppm based on
the rate of feed to the reactor.
Note: The start of Merox Plus addition may be delayed up to 7 days after the
initial start-up of the unit.

6.4.1.4. Catalyst ( Charcoal ) Loading

Prior to the loading of catalyst into the reactor, all internals should be installed
and inspected. The inlet distributor spray pattern should be checked to ensure an
adequate distribution pattern of liquid across the cross-sectional area of the
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Reactor ( 801-R1 ). This should be done with water when the Circulation Pump
( 801-P4A/B ) is run-in.
The Reactor can be loaded with the catalyst only after it has been flushed and
thoroughly inspected again.
The Merox reactor should be isolated from the system, depressured, and the top
and bottom side manways opened. The inlet distributor assembly should be
properly covered to prevent any charcoal from flowing into the distributor during
loading and uncovered after loading. A catalyst hopper with telescopic or
segmented loading sock, that extends approximately to the level of the outlet
collector pipe, is mounted on the top manway for charcoal loading. The sock
position and length are adjusted as the charcoal loading progresses to prevent
any coning or bin effect, which could later cause maldistribution of hydrocarbon
flow through the bed.
During the loading operation, personnel handling the charcoal should wear dust
masks covering the nose and mouth to prevent inhalation of charcoal fines.
After the loading of charcoal has commenced and the bed level is just slightly over
the top of the Johnson Screen collector pipe assembly, charcoal loading should be
stopped. Once the charcoal dust has settled, someone wearing a fresh air pack or
self contained breathing apparatus should enter the reactor via the bottom side
manway to verify that the collector pipe assembly has been completely submerged
with charcoal, and to make certain that there are no unfilled spaces present
underneath any of the laterals. The reactor bottom side manway flange faces
should be checked and a new gasket should be installed. After the manway is
closed, charcoal loading can then be resumed, shortening the sock as loading
progresses.
When the top of the charcoal bed has risen uniformly to within 600 mm of the
inlet distributor, the loading is stopped. Towards the end of the charcoal loading,
the bed depth can be satisfactorily gauged by dropping a probe through the
reactor to manway. After the charcoal dust has settled and the bed is visible, the
top surface of the bed is leveled by hand. Again, the man entering the reactor
must wear a fresh air pack. If necessary, additional charcoal is loaded to provide a
level surface 600 mm below the inlet distributor centerline. A loading diagram
should be prepared showing the appropriate outages and a record should be kept
of the weight, volume, and the type of charcoal loaded.
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6.4.1.5. Alkalinization

The reactor charcoal must now be alkalinized with 10-30o Baume aqueous sodium
hydroxide solution. The caustic concentration is not critical over this range.
However, since the first batch of caustic pumped into the reactor may be diluted
by as much as 50% due to water absorbed by the charcoal, 20o to 30o Baume
caustic can be used as desired.
It is advisable to keep a slight positive pressure of nitrogen on the reactor during
this step to avoid having to air free again before start-up. A nitrogen hose can be
attached to the ¾ inch plugged valve on the reactor vent line for convenience.
Prepare a quantity of 20-30o Baume caustic equal to about 25% of the caustic
settler volume. Close the valves from the reactor side outlet and reactor drain line
to the suction of the Caustic Circulation Pumps (801-P4A/B) and line up the
circulation pump discharge into the reactor inlet line. The reactor drain valve to
the sewer will remain closed for the moment.
Start the Caustic Transfer Pumps (801-P1A/B) at the storage tank ( and the
circulation pump, if necessary ) and begin transferring the caustic into the reactor
at a reasonable rate as indicated by the local flow meter.
As soon as the caustic transfer begins, open the reactor drain valve to the sewer.
As the reactor fills, liquid will be forced out from the reactor drain.
Initially this liquid will be interstitial water displaced by the caustic from the
charcoal. When caustic appears at the drain, as indicated by a quick check of the
specific gravity, close the reactor drain valve. Complete the caustic transfer, then
shut down the pumps and block in the fresh caustic transfer line from storage.
Open the valves in the lines from the reactor side outlet and from the reactor
bottom drain line ( if any ) going to the circulation pump suction. Start the
circulation pump and bring the flow rate up to the rated pump maximum.
Circulate caustic in this manner for a period of at least two hours, preferably
longer. In some cases, it may be necessary to bring additional fresh caustic into
the reactor to maintain suction on the caustic circulation pump during this step.
Stop the caustic circulation pump. The reactor is now prepared to receive feed
kerosene.

6.4.1.6. Realkalinization

During continued operation of a catalyst bed , the feed kerosene will gradually
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wash caustic solution out of the charcoal bed. This caustic will collect in the
Caustic Settler ( 801-V1 ). When the caustic on the charcoal becomes depleted,
mercaptan conversion via the Merox reaction will cease to take place. However,
depletion of the caustic is gradual, not sudden. A regular laboratory analysis
program to determine mercaptan sulfur in the product will show a gradual
increase in mercaptan concentration with time. Since this is largely caused by
loss of alkalinity, it becomes necessary to realkalinize the bed periodically.
Realkalinization is accomplished by pumping the caustic, which has been stored
in the settler, into the feed stream and allowing it to percolate through the bed
along with the hydrocarbon.
Thus realkalinization does not require any interruption in Merox operation. The
recommended circulation rate is 20% of hydrocarbon feed rate. Operation with
excessive caustic circulation rates only results in decreased hydrocarbon
residence time within the catalyst/charcoal bed. Experience indicates that
maintaining this caustic circulation for 30 minutes is adequate for charcoal
saturation. However, the frequency with which realkalinization becomes
necessary will largely depend upon the following:
The degree of difficulty of converting the mercaptans in the particular feedstock.
For a light straight run gasoline, the interval between realkalinizing could be as
long as 30 days, but for a heavy kerosene from a difficult stock, it might be 24
hours.
The amount of surface active material present - both naturally occurring
sulfonates and naphthenates and synthetic corrosion inhibitor additives. For
example, if prewashing to remove naphthenates is inefficient, realkalinizing of
the bed must be done more frequently.
As the same caustic is recirculated over the charcoal bed for alkalinization, it will
tend to collect impurities as they are washed from the bed. With repeated reuse,
the caustic becomes highly discolored. When this occurs the used caustic should
be removed from the Merox unit for disposal and replaced with fresh caustic.
Experience has indicated that caustic can sometimes be reused as many as five
times, but specific refinery experience will dictate caustic consumption.

6.4.1.7. Catalyst Impregnation/Re-impregnation

The impregnation is a procedure whereby the fixed bed catalyst is prepared by

impregnating activated charcoal with Merox FB reagent. Since Merox No. 8 are
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pre-impregnated, they do not require impregnation before the initial start-up. A
carrier solution is used to deposit the catalyst on the charcoal and is recirculated
in order to transfer additional catalyst.
The most economical carrier identified is a 0.2 wt% solution of ammonia dissolved
in water.
The initial catalyst impregnation is performed on fresh charcoal. Sometimes, as a
step relating to the activation process during manufacture, the charcoal is
subjected to acid washing. When this occurs, the residual acidity remaining on
the charcoal will neutralize some of the ammonia added and significantly more
ammonia than expected must be injected to establish the proper carrier ammonia
concentration.
Subsequent impregnations are called reimpregnations. However, the
reimpregnation procedure differs little from the initial impregnation procedure.
It can be used for reimpregnating Merox No. 8 catalyst.
A reimpregnation becomes necessary when hot water washing no longer restores
sufficient catalyst activity or when the frequency of hot water washing required to
maintain acceptable activity becomes impractical. All reimpregnations should be
preceded by hot water washing and neutralization. The following procedure is
employed for catalyst impregnation and reimpregnation.
1. ( This step for reimpregnations only ). Drain the acidified ( 6.5 pH )
neutralization water, opening the reactor top vent line, and displacing this
water with air.
2. Fill the reactor with cold, clean condensate or equivalent quality water,
venting air as necessary. Note: The new charcoal may have a tendency to
float due to its inherently low ABD and also to air trapped in the charcoal
pores.
Periodically, the reactor top manway should be opened to visually see if the
charcoal bed is floating. If the charcoal starts to float, temporarily stop
bringing in water as per Step 3. This will result in the wetting of the charcoal
and in liberation of the air trapped in the pores so that the charcoal will no
longer float. Once the charcoal has settled, resume filling the reactor with
water.
3. When the reactor is full, [ water level 1 foot ( 300 mm ) above inlet
distributor ], begin circulating this water from the reactor outlet collector
assembly back to the inlet distributor via the circulation pump at maximum
rate.
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4. While circulating water, inject ammonia into the pump suction at a minimum
location of 3 meters upstream of the pump. The injection rate should be
sufficiently slow so that the total amount needed will be introduced during
the time it takes to pump the entire water inventory through the system
twice. The ammonia injection rate can easily be monitored by following the
weight loss of an ammonia cylinder mounted on a platform scale. An estimate
of the amount of ammonia required may be calculated as follows:

A = 0.002 W ( T - 0.2L + D/6 ) ( D2/4 )

where:
A = kg of ammonia required
D = Internal diameter of reactor in meters
L = Length of charcoal bed loaded in meters
T = Tangent length of reactor in meters
W = kg/m3 of water

5. When the ammonia concentration has stabilized, verify that it is a minimum

of 0.2 wt% by laboratory analysis. Buffering phenomena encountered when
reimpregnating used charcoal can cause sharp and unpredictable changes in
pH while adding ammonia. Note: If scheduling will permit, the
ammonia/water solution can best be stabilized at a uniform concentration by
continuing circulation overnight. No adverse effects have been experienced
with slightly higher concentrations, other than the odor incurred upon
disposal.
6. Fill the 208 liter catalyst mix drum with a working level of about 114-132
liters of ammonia/water carrier solution.
7. A small air flow should be kept on the air sparger to keep the catalyst
suspended. Excessive air rates can lead to formation of a stable foam.
8. Shake the Merox FB container to disperse any reagent that may have settled
and pour the contents directly into the drum. Do not exceed one kg of catalyst
per 10 liters of carrier solution ( 0.1 kg/liter ). Thus, up to 15 kg ( 6 bottles ) of
Merox FB may be added to the drum at one time. If more catalyst is required,
it should be added in equal batches of no more than 15 kg.
9. Using the circulation pump eductor, slowly educt the catalyst/carrier solution
into the circulation pump suction. Do not exceed a rate of 0.2 m3/hr .
10. After emptying the mix drum, flush it several times with carrier solution and
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educt the reactor in order to get all of the residual catalyst into the reactor.
11. Continue circulating water through the reactor for a minimum of 1 hour
following completion of catalyst addition. Continuing water circulation
overnight may aid in attaining a more even distribution of catalyst on the
charcoal.

12. During both an impregnation and reimpregnation, the carrier exiting from
the reactor outlet may become slightly blue. This should not cause alarm
since as little as 1 wt-ppm dispersed Merox FB reagent will make a liquid
appear blue and 10 ppm will make it very dark blue. Color breakthrough
during the original impregnation is not a common as during a
reimpregnation due to the possibility of incomplete bed washing and/or
acidification. Continued circulation of the reagent/carrier solution over the
bed will often result in complete loss of color in the solution. If the solution
remains an intense blue during an impregnation or reimpregnation,
channeling may be the cause.
 The following procedure has been used successfully to remove channels:
 Block in the reactor inlet and outlet lines.
 Attach an air hose to the connection provided at the outlet collector pipe.
 Inject a full amount of air for no longer than thirty seconds to bubble, or
“fluff” the charcoal bed.
If convenient, an observer should look at the bubble patterns from the top of
the manway. Large, coagulated bubbles would be an indication of channeling.
A uniform bubble distribution would be an indication that channeling no
longer exists.
13. The reactor may now be drained, using air or nitrogen.
14. Open the reactor top manway and obtain an outage measurement from the
top of the catalyst bed to the face of the manway flange.
15. Also, collect 8-10 spot samples of the impregnated charcoal from
predetermined representative positions at the top surface of the reactor bed
so as to enable future determination of the lateral catalyst distribution
profile, if necessary. These samples should be held for analysis in case trouble
indicating maldistribution of catalyst should develop when the unit is put
into operation.
An impregnated/re-impregnated catalyst bed now must be alkalinized.
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6.4.2. Trouble Shooting

Problems may occur in the operation of this unit because of:

 Insufficient Air
 Inadequate alkalinity
 Excessive hydrocarbon feed rate
 Inadequate hydrocarbon temperature
 Presence of interfering impurities ( sulfides )
 Channeling
 Surfactants accumulation
 Normal deactivation
Difficulties arising from most of these are readily apparent as indicated by
improvement following corrective action at the unit, but a few require more
discussion:

6.4.2.1. Air Injection and Reactor Pressure

Sufficient pressure must be maintained at the top of the reactor to completely

dissolve all of the air injected into the hydrocarbon. Failure to do so will result in
the formation of a separate air phase at the top of the reactor. Such an air phase
collecting in the reactor will gradually displace hydrocarbon from the bed. This
will promote channeling when some or all of the hydrocarbon short circuits the
bed. This effect continues even when the air phase is subsequently eliminated.
Channeling essentially reduces residence time resulting in decreased mercaptan
conversion. Therefore, as a part of routine operation, the reactor overhead vent
line should be checked frequently for evidence of a separate air phase. If air is
found, it should be vented. Concurrently, either the reactor pressure should be
increased within mechanical limits or the air injection rate should be decreased in
order to alleviate the problem.

6.4.2.2. Deactivation

Surfactant accumulation on the fixed bed catalyst results in gradual catalytic

deactivation. This is usually the case when Merox treating hydrocarbons of
higher boiling ranges such as kerosene. When the untreated virgin feedstock has
a neutralization number in excess of 0.010 mg KOH per gram of sample, proper
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prewash control is essential to minimize the accumulation of naphthenate salts
on the charcoal/catalyst bed and prevent rapid deactivation. Some feedstocks
contain surfactants which may or may not be indicated by a higher neutralization
number and may not be removed by prewashing. These are additives used in
crude oil production, recovery, and even in processing. An example of the latter is
certain corrosion inhibitors used in fractionation columns.
When catalyst bed deactivation is so severe as to require reduced feed rate,
reactivation is required. See Section 6.4 ( Special Procedures ) for a detailed
description.

6.4.2.3. Residence Time

The residence time, or catalyst contact time, is inversely proportional to the feed
rate. An increased feed rate may not allow sufficient catalyst contact time to
obtain acceptable product quality. Particularly when some deactivation has
occurred.
Mercaptans that are difficult to treat ( higher molecular weight, more highly
branched, etc. ) require more residence time that those that are easy to treat.
Therefore, when the hydrocarbon distillation endpoint is increased, the feed rate
must sometimes be decreased to maintain the same product mercaptan content.
Feed rate reductions might be necessary even if the total mercaptan
concentration decreases. This often occurs when changing crude origins and
introducing feedstock with a high concentration of difficult-to-treat mercaptans.

6.4.2.4. Temperature

Fixed bed sweetening reaction proceeds at normal run down temperatures, 30-45
oC. As discussed earlier, the Merox unit is normally operated at the lowest
temperature that will provide sweetening with a reasonable amount of excess air
( 1.5 to 2.0 times theoretical ). However, as catalyst bed deactivation occurs, it is
possible to raise the normal feed temperature in increments of 3 oC to offset lost
activity until time permits a shutdown and reactivation of the catalyst bed.

6.4.2.5. Realkalinization

Operation of a fixed bed of Merox No. 8 unit requires alkalinization initially, then
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intermittent realkalinization as described in Section 6.4 ( Special Procedures ).
UOP recommends daily recirculation of caustic at 10 to 20 vol-% of feed rate for a
period of 15 to 30 minutes. This will assure adequate alkalinity in the bed
catalyst bed. A regular schedule of testing to monitor mercaptan concentration in
the product will serve to alert operation personnel to the need for more frequent
caustic realkalinization. We recommend that the circulation rate and duration be
kept constant but that frequency be increased to twice daily, then 3 times daily,
and so forth until finally bed reactivation is required.
Some refiners prefer to forego daily caustic circulation and wait until product
mercaptan level rises to an objectionable level before realkalinizing. This
technique is workable for less troublesome feedstocks but will not be as effective
as daily realkalinization in terms of need for bed reactivation.
In either case, rising mercaptan content in the product under otherwise stable
conditions is a good indication that realkalinization is required.

6.5. General Overall shutdown plan

Shutdown can be classified into complete shutdown and emergency shutdown.

The complete shutdown, which means a normal shutdown, is a scheduled
shutdown, while the emergency shutdown is an unscheduled shutdown due to
failure, accident or an unavoidable calamity.
The emergency shutdown procedures are shown in Section 7.
A temporary, or emergency, shutdown may be accomplished on any Merox unit
with the following actions:
1. Stop air injection by closing at least one positive shutoff valve.
2. Divert the hydrocarbon flow to off specification storage facilities upstream of
the Merox unit.
3. Open the Merox unit bypass, if provided, and block in the unit inlet and
outlet valves.
4. As an optional procedure, any caustic pumps in service may be shut off.
A normal shutdown is accomplished in the same manner as a temporary
shutdown. The unit is then emptied following normal refinery safety practices
pertaining to venting, draining, disposing of hydrocarbon, blinding, and
steam-out. Fixed bed units should not be shut down for an extended period of time
while still containing hydrocarbon. Certain polymerization can occur which will
result in decreased charcoal life. If an extended shutdown is planned, the charcoal
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bed should be steamed free of hydrocarbon, hot water washed, and blanketed
with nitrogen to prevent rusting.

6.6. Detailed step-by-step shutdown procedure

1. One shift before shutdown, skim the scum and foggy materials in 801-ME7
for several times. Keep 801-V1 interface at minimum level.
2. Notify the CDU unit to cut off the raw kerosene feed to the unit and divert to
blending header.
3. Stop air injection to 801-ME2 by stopping 801-C1A/B. Divert product to slop.
4. Cut off 3o Be caustic and Merox Plus injection. Stop 801-P2A/B and
801-P3A/B.
5. Cut off power in 801-ME7.
6. Block in the system. Introduce N2 to 801-ME7 vent line and pressure out the
spent caustic in 801-ME7 to Effluent Treatment System. Drain out the
remaining portion to the Oily Water system. Pump out the oil in 801-ME7 to
slop using 801-P4A/B.
7. Introduce N2 to 801-R1 vent line and pump out the oil in 801-R1 to slop using
801-P4A/B. The drain the remaining portion with spent caustic to the
Effluent Treatment System.
8. Introduce N2 to 801-V1 and 801-V3 vent lines and pressure out the spent
caustic in 801-V1 and 810-V3 to Effluent Treatment System. Pump out the oil
in the caustic settler and the wash water using 801-P4A/B and replace it with
condensate using 801-P1A/B.
9. Introduce N2 to the vent lines of the salt filter and clay filter and pump out
the oil to the slop tanks using 801-P4A/B. Note : Admit N2 as necessary to
maintain positive pressure at vessels.
10. Depressure the system to flare and steam out 801-ME7 using Desuperheater
801-ME6.
11. If required, water back washing can be applied on 801-V4 and 801-V5. Use
hot water wash to remove remaining oil in 801-R1.

6.7. Blanking off

Every line connecting to a nozzle on the vessel to be entered must be blinded at

the vessel. This includes drains connecting to a closed sewer, utility connections
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and all process lines. Install additional blinds at the battery limits as necessary
for safety. The location of each blind should be marked on a master piping and
instrumentation diagram (P&ID), each blind should be tagged with a number and
a list of all blinds and their locations should be maintained. One person should be
given responsibility for the all blinds in the unit to avoid errors.

6.8. Opening Equipment

The area around the vessel manways should also be surveyed for possible sources
of dangerous gases which might enter the vessel while the person is inside.
Examples include acetylene cylinders for welding and process vent or drain
connections in the same or adjoining units. Any hazards found in the survey
should be isolated or remove.
Safe access must be provided both to the exterior and interior of the vessel to be
entered. The exterior access should be a solid, permanent ladder and platform or
scaffolding strong enough to support the people and equipment who will be
involved in the work to be performed.
Access to the interior should also be strong and solid. Scaffolding is preferred
when the vessel is large enough to permit it to be used. The scaffolding base
should rest firmly on the bottom of the vessel and be solidly anchored. If the
scaffolding is tall, the scaffolding should be supported in several places to prevent
sway. The platform boards should be sturdy and capable of supporting several
people and equipment at the same time and also be firmly fastened down. Rungs
should be provided on the scaffolding spaced at a comfortable distance for
climbing on the structure.
If scaffolding will not fit in the vessel a ladder can be used. A rigid ladder is
always preferred over a rope ladder and is essential to avoid fatigue during
lengthy periods of work inside a vessel. The bottom and top of the ladder should
be solidly anchored. If additional support is available, then the ladder should also
be anchored at intermediate locations. When possible, a solid support should
pass through the ladder under a rung, thereby providing support for the entire
weight should the bottom support fail. Only one person at a time should be
allowed on the ladder.
When a rope ladder is used, the ropes should be thoroughly inspected prior to
each new job. All rungs should be tested for strength, whether they be made of
metal or wood. Each rope must be individually secured to an immovable support.
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If possible, a solid support should pass through the ladder so that a rung can help
support the weight and the bottom of the ladder should be fastened to a support to
prevent the ladder from swinging. As with the rigid ladder, only one person
should climb the ladder at a time.
Also refer to Section 10.12 “Entering tanks, drums or other vessels.

6.9. Special Precautions

6.9.1. Safely Entering A Contaminated Atmosphere

Under certain conditions, activated charcoal can become an excellent oxygen

scavenger, depleting the oxygen content of the atmospheric air contained in
Merox fixed bed reactor. Therefore, precautions should be taken any time refinery
personnel find it necessary to enter any vessel which contains activated charcoal.
Anyone entering a vessel which contains an inert or contaminated atmosphere
must follow all prescribed standard safety precautions and regulations which
apply. In particular, when entering a reactor containing used charcoal, and which
therefore contains some hydrocarbons, there are a number of additional
precautions that apply and that should not be overlooked. For this discussion, it is
assumed that entry into a reactor containing used charcoal under a nitrogen
blanket is planned.
The following precautions should be included in the standard procedure:
1. The reactor should be isolated by positive action, such as blinding, to exclude
all sources of hydrocarbon, hydrogen, air, etc.
2. Just prior to entry, all purging of nitrogen through the catalyst bed should be
discontinued, and nitrogen purged lines should be inserted at points above
the catalyst bed. This is to assure that there will be no forced flow of vapors
passing upward through the catalyst bed and into the working area.
3. Install an air mover outside the reactor near the open manway nozzle to
sweep away the vapors leaving the reactor.
4. The man entering the reactor must be equipped with a fresh air mask in
proper working condition with a proper air supply.
5. There should be a separate spare air supply that is independent of electrical
power available and ready for immediate use and transfer to the man in the
reactor.
6. The man entering the reactor should wear a safety harness with a properly
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attached safely line.
7. There should be a minimum of two back-up men at the manway nozzle in
continual surveillance of the actions of the man in the reactor.
8. There should be a spare fresh air mask complete with its own separate air
supply to allow a second man to enter the reactor quickly in case of an
emergency. Therefore, this spare equipment must be compact enough to
allow the second man to enter through the manway while wearing the
equipment.
9. It is recommended that any man working in a vessel that is under a nitrogen
blanket not be permitted to descend through any passageway such as tray.
The reason for this precaution is that, should a man develop some difficulty
while below a tray, for example, to the point where he could not function
properly or lost consciousness, it would be extremely difficult for the
surveillance team outside the reactor to pull the man up through the small
tray manway by use of the safety line.
As an added precaution, it is suggested that the man in the vessel have available
to him in the vessel, an emergency self-contained air supply and appropriate
associated equipment. Preferably, the emergency air supply could be connected to
the fresh air mask he is wearing. Such “reserve air supply” systems are available
commercially.
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7. EMERGENCY SHUTDOWN

7.1. General Instructions

An emergency can be caused by the failure of an essential utility ( power, steam,

cooling water, etc. ), by mechanical failure, by a serious leak or by fire.
In these cases a partial or complete shutdown must be carried out quickly but
without damaging equipment.
A partial failure of utility, such as power dip may necessitate a reduction in
throughput without enforcing a shutdown.
At all times the safety of personnel is the overriding consideration.
The operators must judge the conditions of the emergency correctly in order to
take the first necessary action in an actual emergency, and then appropriate
action must be taken according to the changes in the conditions.
If a failure is likely to continue for a considerable time, the unit must be shut
down according to complete shutdown procedure after taking the initial necessary
action.
The basic actions which are to be taken in the event of each type of failure are
described below. Although failures which may occur are infinite in variety typical
large failures are considered because the action to be taken to overcome minor
failures may be inferred therefrom.
Since the Kerosene Merox unit is designed to operate at low pressure and low
temperature, loss of water, power, steam, instrument air for a short duration is
not expected to cause to much interruption to the plant. However, to protect the
catalyst and clay filter, the following actions must be taken:
 Stop the kerosene feed. Cut the power to 801-ME7 and stop caustic and
Merox Plus injection.
 Stop the air injection.
 Bypass clay filter. Lower down the pressure setting on PV-008.
Note: Prolonged soaking of reactor catalysts with kerosene is not advisable. If
shutdown lasts longer than 7 days, the reactor should be cleared of oil and
steamed.

7.2. Fire

If a fire occurs in the plant, that section of equipment in which the fire has
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occurred must be isolated to confine fire and depressured to eliminate the source
of combustible material. Unless the fire is small and can be handled quickly the
plant will shutdown. Operating supervisor on duty will advise on shutdown,
based on refinery procedures in place
The following action shall be taken:
1. Notify the fire/safety section of the refinery.
2. Follow operation supervisor’s orders on shutdown and fire fighting
procedures.
3. If plant must be shutdown:
 Stop the kerosene feed
 Stop the air injection
 Cut the power of the Electrostatic Caustic Prewash ( 801-ME7 )
 Stop all the pumps which are running.
 Run down the kerosene in the plant into the light slop header to reduce
the pressure if possible.

7.3. Power failure

When power failure occurs, all the pumps in the unit and the Air Compressor
System ( 801-C1A/B ) will stop. The Kerosene Product Pumps ( 100-P9A/B ) at
CDU will also stop which will lead to a feed failure. Refer to section 7.7 for the
necessary actions.

7.4. Instrument Air failure

When the supply of instrument air is stopped, the control valves will fail to their
fail safe position to maintain the unit to a safe condition. Therefore all related
pumps should be stopped.

7.5. LP Steam failure

LP steam is intermittently used in this unit for hot water washing of the reactor.
Therefore, there is no serious consequence foreseen except for delays when LP
steam failure occurs.
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7.6. Water failure

7.6.1. Cold Condensate failure

Condensate is used intermittently in this unit, therefore, there is no serious

consequence foreseen when it fails. However, a condensate failure when required
will have an effect on the caustic dilution operation, hot water washing and on the
water wash supply to 801-V3

7.6.2. Cooling Water failure

When the supply of cooling water is stopped, kerosene rundown temperature will
be increased.

7.7. Feedstock failure

When the feed supply of kerosene is stopped, the unit will be put temporarily into
stand-by mode until the feed supply is brought back on line. Failure to restore the
feed supply for a long period of time will cause the unit to shutdown for a while to
protect the catalyst in the reactor.

7.8. Equipment Failure

Major equipment failure ( e.g. 801-R1 ) will cause the unit to shut down for
repairs. Equipment failure at the post treatment section, may or may not
shutdown the operation of the unit dependent on the product being processed.
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8. MAJOR EQUIPMENT AND ITS SERVICE

8.1. Summary Tables

Refer to Attachment 8.1( Equipment List of Kerosene Merox Process Unit, Doc.
No. S-801-1224-101 ).

8.2. Tower summary

Not applicable to this unit.

8.3. Drum summary

8.3.1. Electrostatic Coalescer Prewash ( 801-ME7 )

For those higher boiling, straight run hydrocarbon feedstocks with high
concentrations of naphthenic acids, it is necessary to provide a continuous caustic
prewash equipped with an integral electrostatic coalescer. This vessel is
designed, supplied, and serviced by a vendor specializing in such units; their
operating instructions must be followed. The Electrostatic Coalescer Prewash for
this unit is a horizontal type vessel and uses caustic on a once-through basis.
In principle, dilute caustic and naphthenic acid rich feedstock are mixed in an
adjustable mixing valve, then flow to a gravity separator vessel where caustic
passes to the bottom for disposal and treated hydrocarbon passes to the top.
Droplets of caustic solution and caustic/hydrocarbon emulsion entrained in the
hydrocarbon pass near high voltage electrical grids. This high voltage electrical
field causes the entrained droplets to coalesce and form larger droplets which
eventually fall by gravity to the lower caustic level.
Interfacial skim nozzles are usually provided to draw off sodium naphthenate
soaps.
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Electrostatic Coalescer
Prewash, 801-ME7

Caustic
Washed
Mixing valve Kerosene

LIC
Dilute 303
Caustic

Kerosene
Spent
Caustic

8.3.2. Caustic Settler ( 801-V1 )

The Caustic Settler is a horizontal vessel designed to permit gravity separation of

aqueous caustic solution from the hydrocarbon product. An inlet distributor is
provided to avoid excess inlet turbulence and promote an even flow distribution
through the vessel.

Caustic Settler,
801-V1
Caustic
and Kerosene
Kerosene Outlet

Caustic
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8.3.3. Wash Water ( 801-V3 )

When the product is to be used as an aviation turbine fuel component, product

water washing is typically needed to remove water soluble surfactants that might
otherwise cause failure of water separation related product specifications. This
water washing step will also remove any entrained sodium soaps or caustic
solution. Occasionally, product water washing is used strictly to remove
entrained caustic.
The Wash Water vessel is a vertical type vessel, operated batchwise. Hydrocarbon
enters the bottom of the vessel and jets through a distributor with holes oriented
downward. The distributor hole area and orientation is designed to provide
adequate mixing and should be checked for conformance with the application.
The vessel is normally operated half full of water and is replaced batchwise.
The vessel is also equipped with skim lines near the interface to drain off any
interfacial scum which might accumulate. This scum is usually an emulsion that
forms at the water/hydrocarbon interface and will lead to water carry-over
downstream unless it is drained.
A full diameter stainless steel wire mesh blanket is provided in the upper section
of the vessel below the hydrocarbon outlet to coalesce and remove most of the
entrained water droplets or emulsions. The mesh blanket should be adequately
secured to its support with tie-down wires. Periodic inspections should be
conducted to evaluate mesh blanket integrity.
The Water Wash vessel is normally supplied with two parallel inlet distributors,
one near the bottom and second several feet up. Normal operation utilizes the
bottom distributor. The top distributor, with holes oriented upward, is used only
when it is necessary to change out water. This upward hole orientation allows a
calm water phase essentially free of undissolved hydrocarbon to be withdrawn
from the bottom of the vessel.
Steam condensate is required and is added via a water break tank and a pump.
The Water Break Tank ( 801-V2 ) is a small, atmospheric, vertical type vessel
used as a temporary condensate storage tank when filling. Water change-out is
normally made when the total alkalinity exceeds approximately 0.2 wt% NaOH or
a pH of about 12.5.
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Water Wash,
801—V3
Kerosene
Outlet

Kerosene
Inlet 801-V3

801-V2
LIC
006

Drain
and
Fill Condensate
Inlet

OW
801-P5

8.3.4. Salt Filter ( 801-V4 )

The Salt Filter is a vertical vessel containing a bed of granular rock salt, NaCl. Its
function is to remove free water entrained in a hydrocarbon product plus a small
portion of the dissolved water. It is installed upstream of a product clay filter in
order to protect the clay from premature failure due to free water attack of the
crystalline clay structure.
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As the salt removes water, an aqueous salt brine is formed which gravitates to the
bottom of the vessel for disposal by periodic draining. As aqueous salt brine is
formed, salt crystals dissolve, the solid salt bed settles and eventually must be
replenished. This is normally accomplished by bypassing the vessel from time to
time, opening the top manway, and “topping off” the salt bed with fresh rock salt.
The bed should be checked and replenished before it is 50% consumed. It is
recommended to check the level at three month intervals until a consumption
history is established.

Salt Filter,
801-V4
Kerosene
Outlet

Kerosene
Inlet 801-V4

Drai

The hydrocarbon inlet distributor is designed to allow even flow distribution

( upflow ) and is wrapped with a stainless steel screen to exclude salt. The brine
drain collector is a stainless steel screen pipe of a propriety design.

8.3.5. Clay Filter ( 801-V5 )

The Clay Filter is a vertical vessel containing a bed of Attapulgus or Fullers

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Earth type clay. Its function is to remove oil soluble surfactants, metal
compounds, particulates, corrosion inhibitors, and other compounds which
adversely affect thermal stability or water separation which are related to
product specifications.
The Attapulgus clay specified is 30 x 60 mesh particle size and selected for
efficient, long life performance. The Clay Filter is preceded by a salt filter to
remove free water and some dissolved water. Attapulgus clay is hygroscopic; that
is, free water will cause the crystalline clay particles to soften, forming an
amorphous, mud-like mass which quickly compacts and causes a severe pressure
drop to develop. Clay is replaced when product specification testing dictates it has
lost its adsorptive capacity.
The Clay Filter is provided with a small vent line piped from the top head of the
vessel to a location near the grade with the discharge directed to an oily water
sewer. This vent should be checked frequently for a separate air phase; if present,
the air phase should be vented. A separate air phase which penetrates the bed
will result in channeling and premature clay replacement.
An inlet distributor ( top ) is provided to allow even flow distribution, with holes
oriented upward to prevent impingement on the bed of clay. The outlet collector
pipe assembly ( bottom ) is a Johnson Screen propriety design to retain the clay
yet permit hydrocarbon to pass unrestricted. These slots should be checked
Clay Filter,
initially to verify the correct size and to see that damage has not created larger
openings.
801-V5
During each clay bed change-out, clean the collector pipe assembly to avoid
problems of slot blinding and again verify that damage has not occurred.
From Salt
Filter

801-V5

Treated
Kerosene
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8.4. Reactor summary

8.4.1. Reactor ( 801-R1 )

The fixed bed Reactor is normally a vertical vessel designed to contain the
charcoal bed upon which Merox catalyst is impregnated. Internal equipment is
limited to an upper inlet distributor, lower side outlet collector, and bottom drain
screen. Flow is downward through the bed.
The inlet distributor is designed to provide a uniform lateral flow distribution
over the reactor cross section. The distributor holes should be oriented upward.
The holes in the inlet distributor should be protected from plugging during
charcoal loading by wrapping the distributor with canvass or plastic covering.
The outlet collector and vessel drain pipes are especially constructed, stainless
steel, slotted screens of a propriety design manufactured by Johnson Screen.
These slots should be closely inspected before commissioning to ensure that any
damage serving to open these slots is repaired. Any time charcoal is unloaded,
these screens should be cleaned with a wire brush since charcoal fines collecting
here can often lead to screen plugging problems. All flanges should be checked for
proper caustic resistant gaskets and proper bolt tension.
Reactor,
801-R1

Prewashe
d
K

801-R1

To
Causti
c
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8.5. Fired heater summary

Not applicable to this unit.

8.6. Exchanger summary

Not applicable to this unit.

8.7. Pump summary

8.7.1. Caustic Transfer Pumps ( 801-P1A/B )

The Caustic Transfer Pump is provided to transfer periodically the prepared 10o
Baume caustic solution from the 10o Baume Caustic Storage Tank ( 801-TK1 ) to
the 3o Baume Caustic Storage Tank ( 801-TK2 ) for dilution and to the caustic
users ( i.e. Reactor - 801-R1, DieselMax Unit, Naphtha Hydrotreating Unit, and
Amine Treating unit ).
These caustic pumps are centrifugal type pumps and will be constructed with
Ductile Iron.

8.7.2. Caustic Injection Pumps ( 801-P2A/B )

The Caustic Injection Pump is a proportioning type pump provided to

continuously inject 3o Baume caustic solution to the Electrostatic Coalescer
Prewash ( 801-ME7 ) via the mixing valve to remove naphthenic acids from the
feed.
These injection pumps will be constructed with both steel and stainless steel.

8.7.3. Merox Plus Injection Pumps ( 801-P3A/B )

The Merox Plus Injection Pump is a proportioning type pump provided to supply
periodically the needed Merox Plus reagent ( catalyst activity promoter ) to the
Reactor, 801-R1.
These injection pumps will be constructed with both steel and stainless steel.
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8.7.4. Circulation Pumps ( 801-P4A/B )

The Circulation Pump is operated periodically to circulate ammoniated water

to/from the Reactor, 801-R1, during fixed bed impregnation.
These circulation pumps are centrifugal type pumps and will be constructed with
steel.

8.7.5. Wash Water Pump ( 801-P5 )

The Wash Water Pump is supplied to fill the Wash Water vessel with water via a
water break tank. This pump will be operated intermittently.
This water pump is a centrifugal type pump and will be constructed mainly with
Ductile Iron.

8.8. Compressor summary

The Air Compressor system(801-C1A/B) is installed to supply a compressed air

for Merox reaction. The compressors are of a reciprocated type and one machine is
a spare.
The capacity is 39 Nm3/h and the discharge pressure is 10.59 Kg/cm2G.

8.9. Special equipment summary

Not applicable to this unit.

8.10. List of Instruments

Instruments provided for this unit are listed in “Instrument Schedule for
Kerosene Merox Process Unit, Document No.: S-801-1370-101”.

8.11. Summary of all equipment’s drivers

Refer to Attachment 8.1 ( Equipment List of Kerosene Merox Process Unit, Doc.
No. S-801-1224-101 ).
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8.12. Control Valves

Tag No. Service Failure P&ID No.

Action

801-FV-01 Minimum flow line to 801-TK1 Fail Open D-801-1225-11

4 3

801-FV-00 Air from Air Compressor System Fail Close D-801-1225-11

4 5

801-UV-01 Air Compressor System Shut-off Fail Close D-801-1225-11

5 valve 5

801-LV-30 Spent Caustic to Caustic Header Fail Close D-801-1225-11

3 5

801-LV-00 Cold Condensate to Water Break Fail Close D-801-1225-11

6 Tank 7

801-PV-00 Treated Kerosene to Tankage Fail Close D-801-1225-11

8 8

8.13. Fired Heater

Not applicable to this unit.

8.14. Miscellaneous

Refer to Attachment 8.1( Equipment List of Kerosene Merox Process Unit, Doc.
No. S-801-1224-101 ).
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9. FLOW PLANS AND PLOT PLAN

9.1. PFD, MSD and P&IDs

Refer to the following attachments:

Attachment 9.1 Process Flow Diagram ( D-801-1223-101 )
Attachment 9.2 Material Selection Diagram ( D-801-1223-501)
Attachment 9.3 Piping and Instrument Diagram (D-801-1225-101,
D-801-1225-111 ~118 )

9.2. Design Engineering, utility and safety flow plans

Refer to the following attachments:

Attachment 9.4 Piping and Instrument Diagram ( UFD )( D-801-1225-131 ~ 136 )
Attachment 9.5 Area Classification ( D-801-1380-001 )
Attachment 9.6 Fire Protection System Layout for Process Area
( D-926-1225-003 )
Attachment 9.7 Fire Extinguisher Layout for Process and Utility Area
( D-926-1225-011 )
Attachment 9.8 Arrangement of Gas Detectors for Process Area
( D-926-1225-023 )
Attachment 9.9 Arrangement of Fire Alarm System Equipment for Whole
Refinery Area ( D-926-1225-021 )
Attachment 9.10Layout for Whole Fire Protection System
( D-926-1225-002 )

9.3. Plot Plan

Refer to
Attachment 9.11Plot Plan of KMX/LMX/Amine Units ( D-810-1225-001 )

9.4. Safety Shutdown function charts

Refer to
Attachment 9.12Cause and Effect Chart ( S-801-1371-401 )
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10. SAFETY

To prevent accidents it is of the utmost importance that all personnel be

instructed properly of the following subject;
The leaks and responsibilities of the operators
The methods to accomplish this in a safe manner.
The following safety regulation cover operations of particular concern to the
personnel responsible for the Kerosene Merox Process Unit. They are intended to
supplement any existing general refinery safety regulations which cover all units;
reference should be made to the latter for all points not mentioned below;.
Mechanical craftsmen working on his unit will be governed by their own
departmental safety regulations, but the operator should see that none of the
following safety regulations are violated by mechanical workers.
In addition to specifically defined rules and practices, the exercise of good
judgment by every person involved is essential to safe operation by every person
involved is essential to safe operation. An operator should be alert for any
situation which might present a personnel hazard. It should also be the
responsibility of each person familiar with the plant to warn other workers who
enter the plant of possible hazards they could encounter.
All personnel must know the location and use of safely shower, fire extinguisher,
plant fire alarm, and main isolation valves, fire hoses and hydrants, fire blankets,
gas masks and respirators, and other protective equipment such as hard hats,
rubber gloves, etc.
Soda acid or foam type extinguisher must not be used on fire around electrical
equipment because the water solution will conduct electricity and may aggravate
the difficulty or result in the electrocution of personnel.
Carbon dioxide or dry powder extinguisher may be used safely on electrical fires.
The carbon tetrachloride extinguishers liberate poisonous fumes and should not
be used in a confined space, unless precautions are taken to avoid breathing the
vapors.
Gas masks or breathing apparatus must be worn whenever toxic fumes are
encountered.
Safety hats must be worn when outdoors.
Gloves and goggles or face shields should be worn where toxic or hot vapor or
liquid is encountered, and are recommended for use while samples are being
withdrawn and solutions made up.
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Fire extinguishers must be recharged immediately after use. All steam and water
hose equipment must be put back in place after use. Access to such equipment
must not be obstructed.
Gas masks must have fresh cartridges installed after use.

10.1. Emergency fire plan

The fire protection system of the plant is designed to prevent fire occurrence,
control fire escalation, or extinguish fire within short period of time, assuming
there will be no outside fire fighting assistance, with only one major fire at a time.

10.2. Fire fighting and protective equipment

There are five water hydrants with monitors and live hose reels in the process
area.
Suitable fire extinguisher must be readily available. The area around an
extinguisher or hydrant must be clear so that equipment is readily accessible in
case of emergency.
For details, see the relevant drawing for the fire fighting system.
In case of fire in the process facility, there is a chance that vessels or drums will
fall down because of overheating of the supports. The fire fighting should be done
from the windward.
In order to prevent the spread of fire, it is necessary to cool down near equipment
using the fire water system, special equipment for fire fighting and also fire
fighting trucks.
If the process unit is in operation, it is necessary to shut down the unit according
to the typical steps as follows if possible;
1. Cut feed to the unit.
2. Immediately cut the electric power on the Electrostatic Coalescer Prewash
( 801-ME7 ) and air injection to the Reactor ( 801-R1 ). Stop also all pumps
( water, caustic, Merox plus, etc. ) in operation.
3. In an emergency case, open up at an appropriate time PV-008 to depressure
the system.
4. Line up the kerosene rundown to slop.
5. Sectional isolation should be attempted in case of leakage.
DO NOT EVACUATE any hydrocarbon to atmosphere.
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Refer to “ FIRE PROTECTION SYSTEM LAYOUT FOR PROCESS AREA“,
D-926-1225-003 ( Attachment 9.6) for details.

Fire alarm system

Refer to “ARRANGEMENT OF FIRE ALARM SYSTEM EQUIPMENT FOR
WHOLE REFINERY AREA “, D-926-1225-021 ( Attachment 9.9).
Also, Refer to “FIRE EXTINGUISHER LAYOUT FOR PROCESS & UTILITY
AREA “, D-926-1225-011 ( Attachment 9.7 ).

Fixed Water Monitors

Provision for fixed water monitors shall be per “ LAYOUT FOR WHOLE FIRE
PROTECTION SYSTEM”, D-926-1225-002 ( Attachment 9.10 ).
Fixed water monitors have an effective nozzle range of at least 30 m and a
discharge capacity of 1900 liter per minutes. Monitors are arranged so that any
equipment to be protected may be covered by two fixed monitors with a radius of
at least 30m. Monitors are located approximately 15 m from the equipment being
protected.

Fire Hydrants
The maximum distance between fire hydrants serving the process units shall be
50 meters or less as determined by the equipment served.

Live Hose Reel Stations

Heavy duty hose reels having 40 meters of 32 mm hard booster hose equipped
with 38 mm couplings and contain straight stream/fog nozzle, shall be provided
as means for quick water application by one man.

10.3. Fire Protection

Refer to “LAYOUT FOR WHOLE FIRE PROTECTION SYSTEM”,

D-926-1225-002 ( Attachment 9.10) for details.
Structure steel, Pipe racks, Equipment Supports, main supports of heater are
fireproofed. ( Refer to S-000-13B0-001. )
The following are precautions to avoid fire:
1. Leaking flanges, glands, or broken gauge glasses can release kerosene and
caustic solution to the area, creating a fire hazard. All equipment should be
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tested for leaks before start-up.
2. All systems are to be purged to give a non-explosive atmosphere.
3. Trash and rubbish are a fire and stumbling hazard. Pick it up, an operator
should be proud of a clean unit.
4. Overheating vessels by steam may cause damage to the internal assembly.
5. Spilled oil or chemicals around units or in trenches should be cleaned up at
once.
6. Smoking in the process area can cause fires and explosions. Smoke only in
designated areas.
7. Welding or other work which can cause sparks in the process area can cause
fires and explosions. Make the area safe for such work and obtain the
necessary permit from the proper authorities before commencing work.

10.4. Maintenance of equipment and housekeeping

1. Operating equipment should be checked frequently for signs of leakage,

overheating, or corrosion, so that unsafe conditions may be corrected before
they result in serious consequences. Unusual conditions should be reported
at once.
2. Guard around moving shafts, coupling belts, etc., which have been removed
for repairs to the equipment must be replaced when repair work is completed.
3. Tools, pieces of pipe etc., should never be left lying on platforms or railings of
operation equipment where they can be knocked off and injure someone
below.
4. Access to ladders and fire escapes must be kept clear. Waste material and
refuse must be put in proper locations where they will not offer fire or
stumbling hazards.
5. Liquid spills must be cleaned up immediately. Blanket gas leaks with steam
and immediately report leaks for repair.
6. In the event that electrical equipment does not function properly, notify the
electrical department and stay clear of the equipment until the electrician
arrives.
7. Gas cylinders should be stored so that they cannot fall over. Guard caps must
remain in place over the valves of cylinders which are not in use.
8. Care should be taken when installing scaffolding to ensure that the wooden
boards do not contact hot equipment and that no part is allowed to impair
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free access on operational equipment e.g. ladders, stairways, walkways or
valves. Scaffolding should be removed immediately on completion of the work
in hand.
9. Switch pumps regularly when spares are provided. This will assure start the
spare pump will be ready when needed.

10.5. Repair work

1. Mechanical work around and operating unit must be kept to a minimum, and
the minimum number of men should be used.
2. No mechanical work on the equipment is to be done without a properly
authorized work permit.
3. Safety hats must be worn by all personnel in all areas at all times.
4. No burning, welding, open fires, or other hot work shall be allowed in the
area unless authorized by a work permit. Catch basins, manholes, and other
sewer connections must be properly sealed off to prevent the leakage of gases
which may ignite upon contact with an open flame.
5. No personnel shall enter a vessel for any purpose whatsoever until it has
been adequately purged, blanked off, then tested to ensure freedom from
noxious or inflammable gases and an entry permit issued.
6. When flushing equipment with a fire hose, the fire hose must be equipped
with a check valve to prevent backflow into the fire main.
7. Lines operation at a low temperature might fracture if unduly stressed;
therefore, do not physically strike these lines and avoid operation conditions
which would cause a water hammer to start.
8. Do not use light distillates such as gasoline or naphtha to clean machinery or
for any other cleaning purposes.
9. Equipment should not be left open overnight. At the end of each day’s work
blanks or spades should be installed to prevent entry of flammable materials
due to valve let-by.
10. Welding cylinders should be removed from site to a designate safe area at the
end of each working day.

10.6. Thermal expansion in exchangers

Not applicable to this unit.

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10.7. Withdrawal of samples

Samples shall be withdrawn from the unit only by authorized personnel.

Protective equipment, face masks or goggles, and suitable gloves must be worn
for sampling liquids or solids. A container must never be felled to the brim, in
order to minimize risk of subsequent spillage.
When sampling any product liquids, gloves and goggles will be worn.
When sampling any material, gas or liquid, the sampling line must be flushed
long enough to remove dormant materials to insure that the sample obtained
represents the current stream. Pass enough gas through the sample vessel to
insure the displacement of the purge gas and to adjust the temperature of the
sampler to that the composition is not distorted by condensation or flashing, etc.
When the sample composition is representative of the source material,
undistorted by flash vaporization. Certain classes of samples may require inert
atmospheres , cooling or special carrying devices. Wear approved personal safety
equipment and exercise caution to avoid injuries.

10.8. Safe handling of volatile and toxic materials including catalyst

The safety rules given below are for the protection of life and limb, and the
prevention of property loss. It is expected that refinery people will exercise
common sense, alertness, and good judgment in carrying them out. If ever there is
any doubt as to the safety aspect of a particular operation, consult your
supervisor immediately.

10.8.1. Respiratory Protection

Refer to Attachment 9.10 “ ARRANGEMENT OF GAS DETECTORS FOR

PROCESS AREA” ( D-926-1225-023 ).
Most refinery gases, other than air, are harmful to human beings if inhaled in
sufficient concentration. Toxic gases may be classified as either asphyxiating or
irritating. Asphyxiating gases may cause death by replacing the air in the lungs
or by reaction with the oxygen carried in the blood; examples are hydrogen sulfide
carbon monoxide, and smoke. Irritating gases may cause injury or death not only
by asphyxiating but also by burns internal and external/ examples are chlorine
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and sulfur dioxide.
To guard against the inhalation of harmful gases:
 Secure a gas test certificate showing the gas condition of the vessel is safe for
entry.
 Stand on the windward side of an operating from which gases escape.
 Provide proper ventilation.
 All personnel should become familiar with the accepted method of artificial
respiration in order to render assistance to any one overcome by gas, electric
shock, or drowning.
If anyone is overcome by gas, his rescuer should:
 Never attempt a rescue unless an assistant is standing by.
 Protect himself before attempting a rescue by wearing breathing apparatus.
 Get the victim to fresh air as soon as possible.
 Give artificial respiration and send his assistant to call for medical aid.
When using a breathing apparatus, be sure that the mask fits the face properly.
Test it by the approved test method.
Wear the correct type of breathing apparatus, suited to the situation encountered.

10.8.2. Breathing Apparatus ( B. A. )

There are four types of breathing apparatus in general refinery service. They are
the canister type mask, the fresh air hose line B. A., the compressed air
self-contained B. A. and the compressed air line trolley B. A.
1. The canister type mask utilizes a filter element to absorb the poisonous gas
from the air and is used only by personnel working at the TEL/TML building
off/on loading.
Use this mask only in the open air or where the gas concentration is less than
2%, not in a tank or other confined space. A canister type mask does not
protect the user against a deficiency of oxygen. A lifeline should be used in
questionable locations.
When a seal is removed from a canister, mark the date on the canister, and
after one year discard it regardless of how little it has been used.
A record of the amount of time that the canister has been used must be kept
on a tag attached to the canister. Do not exceed the permissible time limit for
the particular canister being used. Inform Safety Department when time
limit is near.
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2. The fresh air hose line breathing apparatus has a length of air hose though
which the wear draws in the air required for respiration.
When a man must enter a tank, sewer, or other confined area where the
atmosphere is 20% or more of the lower explosive limit, or contains evidence
of hydrogen sulfide or other toxic materials, a fresh air breathing apparatus
must be used. It is to be used subject to the following conditions:
 The free end of the air hose line must be placed where only fresh air can
enter it, but not more than 100 meter of hose should be used.
 A life belt and rope should always be used with the end fixed so that it
will not fall back into the tank or sewer.
 Be sure that the harness is buckled close to the wearer’s body so that it
will not slip over his shoulders if a rope rescue is necessary.
3. The compressed air self contained breathing apparatus has a self-contained
air supply carried on the back of the user. It is one of two of the four types
that is completely independent of outside air.
It is used principally in emergencies.
After use, always notify the proper department so that they can recharge the
cylinders as soon as possible.
4. Compressed air line trolley breathing apparatus. This breathing apparatus is
also completely independent of outside air. It is principally used where the
fresh air line breathing apparatus would be unsuitable.

10.8.3. Corrosive Materials

Whenever containers of corrosive chemicals such as ammonia, chlorine, caustic

soda, sulfuric acid, etc., are to be opened or emptied, always have a connected
water hose handy to flush off and help absorb spilled material and to reduce
spread of toxic vapors.

10.8.4. Poisonous Materials

10.8.4.1.Sodium Hydroxide ( NaOH Caustic Soda )

Refer to the appropriate safety bulletin published by the National Safety Council
or the Manufacturing Chemists’ Association.
Caustic solution, commonly called lye, and technically known as sodium
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hydroxide, is used so widely in petroleum refining, that its potential hazards are
often carelessly overlooked. Certain general precautions should be observed.
Goggles or face shields should be worn at all times in the processing area. Painful
injury and possible blindness can result if caustic reaches the eyes. A bubbler
fountain should be provided for the purpose of washing the eyes if an accident
should occur. Boric acid solution should be available for first aid after washing
the injured eye with copious quantities of water. All eye injury cases, even slight,
should be referred to a physician.
Workmen should be impressed that caustic does not give immediate warning of
its presence on the skin by burning or irritation, as in the case of many other
chemicals. A severe burn can result from caustic before the individual realizes its
presence on the skin. However, the presence of caustic on the skin before burning
sensation develops can be recognized by its slippery and soapy feeling. A
physician should be consulted in case of a severe skin burn. Some refiners keep a
tub of diluted vinegar handy to neutralize caustic on tools, rubber gloves, etc.,
after washing in water.
In view of the foregoing, workmen should be instructed to wear, in addition to face
shields or goggles, rubber gloves and rubber aprons when performing any work
which exposes them to caustic. Depending upon conditions, it may be advisable to
wear protective rubber footwear, as caustic is destructive to leather. Incidentally,
cotton material is more resistant to caustic than wool, and therefore is preferable
for clothing. Although it should not be considered as a protective material.
Total(overall) rubber clothing is preferable in all cases.
When caustic has come into contact with the skin, the area should be immediately
flushed with water for several minutes, and depending upon the severity of the
exposure, this an be followed by a two percent acetic acid wash to neutralize any
last traces of caustic. Facilities for quick action in the matter of water washing
should be available.
A treadle operated safety shower equipped with a quick opening valve should be
installed in the area. In cold seasons provisions should , of course, be made to
supply with warm water.

10.8.4.2.Catalyst

While Merox catalyst has no apparent harmful effect on the skin, sensitive
individuals may be affected and prudence dictates that catalyst should not be
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permitted to contact the skin. If such contact should result, that catalyst should
be carefully washed off with copious quantities of soap and water until the blue
color can no longer be detected. A mechanic’s waterless skin cleaner may also be
used to decontaminate the skin.
In no case should Merox catalyst be taken internally. Persons handling Merox FB
catalyst are advised to wear proper protective clothing, rubber gloves, and
splash-proof safety goggles. Decontaminate protective clothing after each use.
Workmen should shower after handling this product before dressing in clean
work clothes or street clothing.

10.8.4.3.Acetic Acid

Acetic acid ( CH3COOH ) is a colorless water-like liquid that has a piercingly

sharp, vinegary odor and burning taste.
Acetic acid solutions in water or organic solvents can be very strongly corrosive to
the skin, and cause irreparable scarring of tissues of the eyes, nose, or mouth.
Any solution containing more than half acetic acid should be considered a
corrosive acid. Its action is insidious because there is no immediate burning
sensation upon applying the strong acid to the unbroken skin and blisters appear
within 30 minutes to 4 hours. Ordinarily, little or no pain is experienced; but
when sensory nerve receptors are attacked, severe and unremitting pain is felt.
After the blisters appear, washing with water or bicarbonate seldom alleviates
the pain. Medical care should be sought immediately. Particular care ought to be
taken in handling acetic acid to avoid spilling on the skin or clothing, or breathing
the vapors. When exposed, wash the acetic acid away with large amounts of water
or dilute sodium bicarbonate solution. Leave areas where the odor of acetic acid
vapor is noticeable.

10.8.4.4.Ammonia

Ammonia is used in the reactor fixed bed catalyst impregnation procedure. Refer
to appropriate safety bulletin published by the National Safety Council or the
Manufacturing Chemist’s Association.
Anhydrous ammonia ( NH3 ) is an extremely toxic chemical which exists as a gas
at ambient conditions and is easily dissolved in water to form ammonium
hydroxide ( NH4OH ), commonly called aqua ammonia.
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Fortunately it has a very pungent odor, which is detectable in concentrations
beginning at about 50 ppm. Exposure, even for short periods, to higher
concentrations can lead to irritation of the throat and eyes and eventually can
become fatal. Therefore, even short-term exposure should be avoided if odor is
detected. Personnel should vacate a contaminated area at the first sign of any
irritation of the throat.

10.9. Preparing for entering process equipment

Anyone entering a vessel which may contain an inert or contaminated

atmosphere must follow safety precautions and rules which apply. The vessels
may contain H2S or other toxic material in addition to hydrocarbons.
Therefore, the following precautions should be included in the standard
procedure.
1. The vessels should be isolated by positive action, such as blinding, to exclude
all sources of hydrocarbon, fuel gas, steam, air, etc.
2. The refinery safety officer and supervisory personnel will give their
permission for vessel entry after they have made the appropriate tests.
3. Install an air mover outside the vessel to sweep away any vapors.
4. The man entering the vessel must be equipped with a fresh air mask in
proper working condition, with a fresh air supply.
5. There should be available and ready for immediate use and transfer to the
man in the vessel, a separate air supply which is independent of electrical
power.
6. The man entering the vessel should wear a safety harness with properly
attached safety line.
7. If the work involves a large distance above the floor of the vessel, scaffolding
or support flooring must be built to prevent dangerous falls.
8. There should be a spare fresh air mask complete with its own separate air
supply, to allow a second man to enter the reactor quickly in case of an
emergency. This spare equipment must be compact enough to allow the
second man to enter through the manway while entering the equipment.
The API publication “Guide for Inspection of Refinery Equipment” or the NIOSH
publication No. 87-113; “A Guide to Safety in Confined Spaces” can be referred to
for additional information on safety procedures for vessel entry and accident
prevention measures.
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10.10. Opening equipment

Every line connecting to a nozzle on the vessel to be entered must be blinded at

the vessel. This includes drains connecting to a closed sewer, utility connections
and all process lines. The location of each blind should be marked on a master
piping and instrumentation diagram ( P&ID ), each blind should be tagged with a
number and a list of all blinds and their locations should be maintained. One
person should be given responsibility for the all blinds in the unit to avoid errors.
The area around the vessel manways should also be surveyed for possible sources
of dangerous gases which might enter the vessel while the person is inside.
Examples include acetylene cylinders for welding and process vent or drain
connections in the same or adjoining units. Any hazards found in the survey
should be isolated or removed.
Safe access must be provided both to the exterior and interior of the vessel to be
entered. The exterior access should be a solid, permanent ladder and platform or
scaffolding strong enough to support the people and equipment who will be
involved in the work to be performed.
Access to the interior should also be strong and solid. Scaffolding is preferred
when the vessel is large enough to permit it to be used. The scaffolding base
should rest firmly on the bottom of the vessel and be solidly anchored. If the
scaffolding is tall, the scaffolding should be supported in several places to prevent
sway. The platform boards should be sturdy and capable of supporting several
people and equipment at the same time and also be firmly fastened down. Rungs
should be provided on the scaffolding spaced at a comfortable distance for
climbing on the structure.
If scaffolding will not fit in the vessel a ladder can be used. A rigid ladder is
always preferred over a rope ladder and is essential to avoid fatigue during
lengthy periods of work inside a vessel. The bottom and top of the ladder should
be solidly anchored. If additional support is available, then the ladder should also
be anchored at intermediate locations. When possible, a solid support should
pass through the ladder under a rung, thereby providing support for the entire
weight should the bottom support fail. Only one person at a time should be
allowed on the ladder.
When a rope ladder is used, the ropes should be thoroughly inspected prior to
each new job. All rungs should be tested for strength, whether they be made of
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metal or wood. Each rope must be individually secured to an immovable support.
If possible, a solid support should pass through the ladder so that a rung can help
support the weight and the bottom of the ladder should be fastened to a support to
prevent the ladder from swinging. As with the rigid ladder, only one person
should climb the ladder at a time.

10.11. Working in columns or vessels

It is recommended that any man working in a vessel which has an inert or

contaminated atmosphere not be permitted to move too far away or into any tight
areas, such as through a column tray manway. The reason for this precaution is
that should the man develop some difficulty while below a tray, for example, to a
point where he could not function properly or lost consciousness, it would be
extremely difficult for the surveillance team outside the vessel to pull the man up
through the small tray manway by use of the safety line.
Any one working in the bottom of the column or vessel should be aware of the
hazard of falling objects. Hard hats should be worn , but these will not provide
total protection against heavy objects. The workmen should be warned to pay
attention, to look, and listen. The maintenance supervisor should be careful when
scheduling work, to avoid having people in the bottom of the vessel when there is
heavy work going on in the top of the column or vessels.
A communication system should be provided for the manway watch so that they
can quickly call for help in the event that the personnel inside of the vessel
encounter difficulty. A radio, telephone, or public address system is necessary for
that purpose.

10.12. Entering tanks, drums or other vessels

Before entering a vessel, the refinery’s safety precautions should be observed.

These usually include the following: sampling the vessel for toxic vapor
concentrations( must be zero) and oxygen concentration( should be min. 17 vol %),
wearing a safety harness, and having an attendant outside the vessel.
An unattended vessel should never be entered.
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10.13. Procedure for removing safety valves

Before removing the safety valve, it is required to confirm that both side of
isolation valve are blocked and depressured safely. It is also required to confirm
that the set pressure of spare safety valve is properly adjusted on the testing
facility in warehouse and block valve of both inlet and outlet line in field are
car-sealed-open.

10.14. Work permit procedure and work permit format

Before entering the vessel, a vessel entry permit must be obtained. A vessel entry
permit insures that all responsible parties know that work is being conducted
inside of a vessel and establishes a safe preparation procedure to follow in order
to prevent mistakes which could result in an accident The permit is typically
issued by the safety engineer or by the shift supervisor.
The permit should be based on a safety checklist to be completed before it is
issued. The permit should also requires the signatures of the safety engineer, the
shift supervisor, and the person that performed the oxygen toxic and explosive
gas check on the vessel atmosphere. Four copies of the permit should be provided.
One copy goes to the safety engineer, one to the shift supervisor, one to the control
room, and one copy should be posted prominently on the manway through which
the personnel will enter the vessel.
The permit should be renewed before each shift and all copies of the permit
should be returned to the safety engineer when the work is complete. Additional
requirements or procedures may be imposed by the refiner, but the foregoing is
considered the minimum acceptable for good safety practice.

10.15. Operation notes relating to HAZOP review

Refer to “HAZOP STUDY REPORT”, S-801-1220-101 and “HAZOP ACTION

FOLLOW-UP LIST”, S-801-1220-102.

Action Recommendation Oper. Manual

No. Section No.
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3 Operating manual includes a step by step 5.2 , 5.3 , 6.2,

procedure 6.6
for safety start-up and shut down of 801-ME7.

10.16. Material Safety Data Sheet ( MSDS ) of all the chemicals, catalysts, etc.

Later on.
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11. MISCELLANEOUS

11.1. Conversion Tables

English - Metric Conversions and Abbreviations

Multiplied
English Unit Abbr. By . Metric Unit Abbr.

length inch in 25.4 millimeter mm

foot ft 304.8 millimeter mm

area square foot ft2 0.09290 square meter m2

volume cubic foot ft3 0.02832 cubic meter m3

standard cubic SCF 0.02826 standard cubic std m3
feet of gas* meters of gas
gallon gal 0.003785 cubic meter m3
barrel bbl 0.1590 cubic meter m3

temperaturedegrees Fahrenheit OF OC=5/9(OF-32)degrees Celsius OC

pressurepound per square inch psi 6.895 kilopascal kPa

inch of mercury at 32ºF in Hg 0.1333 kilopascal kPa
inch of water at 4ºC in H2O 0.2491 kilopascal kPa
pound per square inch psi 0.07030 kilograms per kg/cm2
square centimeter

mass pound mass lb or lbm 0.4536 kilogram kg

energy British Thermal Unit Btu 1.055 kiloJoule kJ

power horsepower hp 0.746 kilowatt kW

British Thermal Btu/hr 0.2931 watt W
Units per hour

*UOP calculates standard cubic feet of gas at 60º F and 14.696 psia. UOP proposes to
calculate standard cubic meters of gas at 15º C and 101.325 kPa.

11.2. General Pre-start up procedures

Refer to S-xxx-xxxx-xxx.(Hold)

11.3. Overall start-up and shutdown outlines

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11.4. Offsite systems

The following feed and products are supplied or sent from / to the existing / off-plot
facilities:

No. Stream From To Line Number

1 Treated 801-V5 945-TK22/23/24 801-6”-PL-1803-A1A1
Kerosene
2 Treated 801-V5 Jet Fuel Blending 801-6”-PL-1806-A2A1
Kerosene System

11.5. Catalyst and Chemical Loading / Unloading

Refer to Section 6.4.1.4. ( Catalyst Loading ).

11.6. Catalyst and Chemical Requirements

See Attachment 1.2 ( Catalyst and Chemical Summary, Doc. No.

S-801-1223-502 ).

11.7. Analytical Plan

11.7.1. General Procedure

The ultimate objective of petroleum refining is to produce product hydrocarbon

streams which meet all specifications required for their ultimate end use. To
accomplish this objective, it becomes necessary to characterize the important
physical and chemical properties of the various refinery streams utilizing specific
laboratory analytical testing procedures.
Thus, satisfactory refinery operation depends largely upon proper analytical
procedures for quality control. An analytical quality control program requires five
steps as outlined.
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11.7.1.1.Sampling

The initial objective must be to obtain a characteristic sample of the particular

product stream. Depending upon the properties of the product in question,
specialized techniques may be necessary to obtain a proper sample. UOP method
516 outlines the general techniques recommended for obtaining an air free
sample, an important consideration in control of chemical treating process units.
The sample point itself should be located at a point where no unusual conditions
exist. This normally requires a sample point location in a vertical run of pipe or
from the side of a horizontal run of pipe.
The refinery operation should be steady and free from fluctuations.
The sample point should be well purged to eliminate aged materials, water, dirt,
etc., and to assure withdrawal of a sample representative of the material in the
pipe at that point in time. The sample container must be adequate for the
analysis to be obtained.
The above by no means is intended to be a comprehensive discussion of sampling;
we refer to those who are intrigued by this subject to the excellent publications of
organizations such as API, NPRA, and ASTM. Rather, we want to introduce the
refinery operations staff to some of the basic considerations needed to obtain the
best sample possible.

11.7.1.2.Sample Preservation

Once a proper sample has been obtained, it must, if possible, be preserved intact
until it can be analyzed. This requires the prevention of any physical or chemical
changes in the sample. Changes, particularly chemical, can occur as a result of
many factors. Some of the most perplexing changes have later been traced to
influences of the sampling equipment and container. Often a sample may be
inherently unstable, requiring immediate analysis. Others can be stabilized by
the addition of a passivating compound or preservative. Some specific conditions
to be avoided are as follows:
Do not use plastic containers.
Never use copper or copper alloys including tubing, valves and fittings.
Avoid exposure to light by using amber glass sample bottles.
Avoid exposure to heat.
Minimize exposure to air by using N2 or CO2 purged containers.
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11.7.1.3.Analysis

Follow the analytical method PRECISELY. Each method represents the end
result of many hours of study, testing, and experience. The methods often note
appropriate precautions indicating potential problems to be avoided.
Laboratory apparatus and equipment must be properly calibrated and rechecked
frequently.

11.7.1.4.Error

There are two terms with which one may qualify an analytical result - precision
and accuracy.
Precision refers to the dispersion, or spread, of results. One must consider both
repeatability (duplicate results by same analyst) and repeatability (duplicate
results by different analysts) of results in order to determine the permissible
tolerance in each specification. A higher degree of precision usually requires
minimizing the random experimental error during development of the method.
Accuracy refers to the deviation between a reported analytical result and the true
value. It is accuracy which can be the most damaging since it is normally the
result of systematic error. If any of the above procedures have been compromised,
the effect is always seen in the accuracy of the value reported.

11.7.1.5.Significance

The significance or interpretation of the result obtained is the final step in any
analytical procedure. Misinterpretation of the result would render the whole
procedure useless. Therefore this step is the most important. Often several
analyses measuring different properties may be related to a common
characteristic ( physical or chemical ). Proper analytical procedure should lead to
supporting rather than conflicting conclusions. In attaching appropriate
significance to the analysis, one must consider and relate all of the previous steps
of the analytical procedure to the operation of the process unit. A firm
understanding of the process and its capabilities is essential. From a thorough
application of these five steps, the necessary changes in operation may be
implemented in order to reach the ultimate objective of meeting the necessary
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product specification.
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11.7.2. Analytical Schedule

Analytical Plan

Refer to the operating manual for Laboratory regarding procedures to operate

laboratory equipment and special precautions to chemicals, S-000-1230-xxx
(Later).

Sample Schedules

Recommended sampling requirements are provided in the table below. Test

frequency shown is a rough figure and will be optimized with experience in plant
operation.

(1) Kerosene Feed (801-SN1)

Item Test Method Normal Start-up

SpGr ASTM D-1298 As As
req.(1) req.(1)
Distillation ASTM D-86 As As
req.(1) req.(1)
Acid number ASTM D 3242 As As
req.(1) req.(1)
H2S UOP 163 As As
req.(1) req.(1)
Mercaptan sulfur UOP 163 As As
req.(1) req.(1)
Sulfur ASTM D-1266 or D-4294 As As
req.(1) req.(1)
Color(Saybolt) ASTM D-156 As As
req.(1) req.(1)
Note (1) This stream is the same as kerosene product stream in unit 100.
A sample will be normally taken from 100-SN10.

(2) Kerosene after Prewash (801-SN2)

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Item Test Method Normal Start-up

Acid number ASTM D 3242 1/D 1/D

(3) Kerosene @ Reactor Inlet (801-SN3)

Normally no teat is required.

(4) Kerosene @ Reactor Outlet(801-SN4)

Normally no teat is required.

(5) Kerosene after Caustic Wash (801-SN5)

Item Test Method Normal Start-up

Doctor test (*) UOP 41 or ASTM D 4952 3/Shift 3/Shift
Mercaptan sulfur UOP 163 1/D 1/D

(6) Kerosene after Water Wash (801-SN6)

Item Test Method Normal Start-up

Water separation ASTM D-3948 As req. As req.
characteristics
Jet fuel thermal oxidation test ASTM D-3241 As req. As req.

(7) Kerosene after Salt Filter (801-SN7)

Item Test Method Normal Start-up

Appearance and color Visual As req. As req.

(8) Kerosene after Clay Filter (801-SN8)

Item Test Method Normal Start-up

Water separation ASTM D-3948 As req. As req.
characteristics
Jet fuel thermal oxidation test ASTM D-3241 As req. As req.
Color(Saybolt) ASTM D-156 As req. As req.
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Copper strip corrosion ASTM D-130 As req. As req.

Silver strip corrosion IP-227 As req. As req.
Acid number ASTM D-3242 As req. As req.
Water reaction ASTM D-1094 As req. As req.
Mercaptan sulfur - - -
Sodium+ - - -
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(9) Spent Caustic from Electrostatic Coalescer Prewash (801-SN9)

Item Test Method Normal Start-up

SpGr UOP 210(hydrometer) 1/D 1/D
Total alkalinity UOP 210 1/D 1/D
Percent spent UOP 210 1/D 1/D

(10) Spent Caustic from Caustic Settler (801-SN10)

Item Test Method Normal Start-up

SpGr UOP 210(hydrometer) 1/D 1/D
Total alkalinity UOP 210 1/D 1/D
Percent spent UOP 210 1/D 1/D
Appearance and color Visual As req. As req.

(11) Washing Water in Water Wash(801-SN11)

Item Test Method Normal Start-up

pH pH meter 1/D 1/D
Total alkalinity UOP 210 1/D 1/D

(12) 10 Be’ Caustic in 801-TK1(801-SN12)

Item Test Method Normal Start-up

SpGr UOP 210(hydrometer) 1/D 1/D

(13) 3 Be’ Caustic in 801-TK2(801-SN13)

Item Test Method Normal Start-up

SpGr UOP 210(hydrometer) 1/D 1/D

(*) Done by operators at the unit

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Attachment List of Operating manual for Kerosene Merox Process Unit

Attachment 1.1 Utility Summary ( S-801-1223-501 )

Attachment 1.2 Catalyst and Chemical Summary ( S-801-1223-502 )
Attachment 3.1 Alarm and Trip Schedule ( S-801-1371-102 )
Attachment 8.1 Equipment List (S-801-1224-101)
Attachment 9.1 Process Flow Diagram ( D-801-1223-101 )
Attachment 9.2 Material Selection Diagram
( D-801-1223-501)
Attachment 9.3 Piping and Instrument Diagram ( D-801-1225-101,
D-801-1225-111 ~118 )
Attachment 9.4 Piping and Instrument Diagram ( UFD )
( D-801-1225-131 ~ 136 )
Attachment 9.5 Area Classification
( D-810-1380-001 )
Attachment 9.6 Fire Protection System Layout for Process Area
( D-926-1225-003 )
Attachment 9.7 Fire Extinguisher Layout ( D-926-1225-011 )
for Process and Utility Area

Attachment 9.8 Arrangement of Gas Detectors for Process Area

( D-926-1225-023 )
Attachment 9.9 Arrangement of Fire Alarm System Equipment
( D-926-1225-021 )
for Whole Refinery Area
Attachment 9.10 Layout for Whole Fire Protection System ( D-926-1225-002 )
Attachment 9.11 Plot Plan of KMX/LMX/Amine Units
( D-810-1225-001 )
Attachment 9.12 Cause and Effect Chart ( S-801-1371-401 )
Attachment 10.1 Material Safety Data Sheet ( LATER )