IGS-R-CH-052(0)
June 2012
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IGS
Mercaptan Oxidation Catalyst
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N.I.G.C.
June 2012
IGS-R-CH-052(0)
FOREWORD
This standard is intended to be mainly used by NIGC and
contractors and has been prepared on interpretation recognized
standards, technical documents, knowledge, backgrounds and
experiences in gas industries at national and international levels.
Iranian gas standards (IGS) are prepared, reviewed and
amended by technical standard committees within NIGC
Standardization division and submitted to the NIGC's
"STANDARDS COUNCIL" for approval.
IGS Standards are subject to revision, amendment or withdrawal,
if required, thus the latest edition of IGS shall be
checked/inquired by NIGC users.
This standard must not be modified or altered by the end users
within NIGC and her contractors. Any deviation from normative
references and / or well known manufacturers specifications
must be reported to Standardization division.
Any comments from concerned parties on NIGC distributed IGS
are welcome to technical standards committees and will receive
serious attention and consideration should a revision to
standards is recommended .
GENERAL DEFINITIONS:
Throughout this standard the following definitions, where
applicable, should be followed:
1- "STANDARDIZATION DIV." has been organized to deal with
all aspects of industrial standards in NIGC. Therefore, all queries
for clarification or amendments are requested to be directed to
mentioned div.
2- "COMPANY": refers to national Iranian gas company.
3- "SUPPLIER": refers to a firm who will supply the service,
equipment or material to IGS specification whether as the prime
producer or manufacturer or a trading firm.
4- "SHALL ": is used where a provision is mandatory.
5- "SHOULD": is used where a provision is advised only.
6- "MAY": is used where a provision is completely discretionary.
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N.I.G.C.
June 2012
IGS-R-CH-052(0)
TABLE OF CONTENT
1. SCOPE
1
2. REFERENCE
1
3. DEFINITION
1
4. SYSTEM DESIGN
2
5. QUALIFICATION PROCEDURE
2
6. QUALITY ASSURANCE
2
7. APPLICABILITY
2
8. SAMPLES
3
9. INSPECTION
3
10. MARKING
4
11. PACKAGING
4
12. STORAGE LIFE
4
13. DOCUMENTATION
4
ANNEX A – Mercaptan Oxidation Catalyst Typical Properties
5
ANNEX B – Catalyst Data Sheet
6
ANNEX C – Mercaptan Removal Unit Data
7
ANNEX D – Gas Treating Plant Data
8
ANNEX E – Propane/Butane/LPG Treating Plant Data
13
ANNEX F – Test Methods
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N.I.G.C.
June 2012
IGS-R-CH-052(0)
1. SCOPE
This standard specification provides the technical procedure for selection/substitution
new mercaptan oxidation catalyst that is used for removing mercaptans from natural
gas, LPG, butane and propane.
2. REFERENCE
Throughout this standard specification the following standard is referred to. The
editions of this standard that is in effect at the time of issues of this standard
specification (2012) shall, to the extent specified herein, form part of this standard
specification. The applicability of changes in standard that occur after the date of this
standard specification shall be mutually agreed upon by the purchaser and the
manufacturer/supplier.
ISO 9001 (2008) "Quality Systems – Model for Quality Assurance in Design,
Development, Production, Installation and Servicing”
3. DEFINITIONS
3.1 Mercaptan Oxidation Catalyst
It is a proprietary catalytic chemical process used in natural gas, LPG, butane and
propane processing plants to remove mercaptans by converting them to liquid
hydrocarbon disulfides.
3.2 Extraction Unit
A gas extraction unit is normally consisting of a combination column that includes
prewash, extraction and water wash section while for liquids is normally including
only an extractor column.
3.3 Regeneration Unit
A caustic regeneration system will convert the extracted mercaptans to disulfide oil
that is separated and removed while the regenerated caustic is returned to the
extraction unit.
3.4 Technical Approved
The technical approved is the first step for qualification of catalyst which technical
information has been evaluated and approved by technical division.
3.5 Laboratory Approved
The laboratory approved is the second step for qualification of catalyst which has
passed laboratory tests.
3.6 Test Field Approved
The test field approved is the third step for qualification of catalyst which has passed
the operational test.
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June 2012
IGS-R-CH-052(0)
4. SYSTEM DESIGN
The manufacturer/supplier shall submit catalyst to be able oxidation of mercaptans to
disulfides in mercaptan removal units as specified in Annex C.
The manufacturer/supplier shall give full details of the proposed catalyst including
chemical base and its characteristics as mentioned in Annex B.
Note: Annexes D and E show typical questionnaires for mercaptan oxidation catalyst
evaluation.
5. QUALIFICATION PROCEDURE
The manufacturer/supplier shall pass following steps respectively as well as all
requirements of this standard specification:
5.1 Technical Approved (Step 1)
The manufacturer/supplier of catalyst shall provide information including original
technical catalogue, MSDS and manufacturing product data sheet. The technical
division shall evaluate information. The catalyst shall be approved by technical
division.
5.2 Laboratory Approved (Step 2)
The manufacturer/supplier that approved by technical division shall provide sufficient
sample for laboratory tests. The laboratory tests will consist of laboratory tests which
are performed in local laboratory and/or accredited laboratory. The catalyst shall be
passed these tests.
Note: Laboratory tests are given in Table A-1 of Annex A. Table A-1 provides typical
properties for catalysts that have been used in natural gas refineries and presents guidelines
for establishing minimum requirements for entering to step 3.
5.3 Field Test Approved (Step 3)
The manufacturer/supplier that passed laboratory tests shall provide sufficient
amount of catalyst for a 90 days period of operational test. The catalyst shall be
passed operational test.
6. QUALITY ASSURANCE
The manufacturer/supplier shall set up and maintain a quality assurance system for
product supplied. The purchaser shall have the right to undertake inspection and
testing of the products to ensure compliance with requirements of this standard
specification.
7. APPLICABILITY
The catalyst shall be easily applicable when used for loading into the system without
any impractical effort.
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June 2012
IGS-R-CH-052(0)
8. SAMPLES
8.1 Laboratory Test Sample
Laboratory test sample shall consist of sufficient amount of catalyst that shall be
forwarded to the purchaser for laboratory tests. Samples shall be plainly identified by
attached durable tag marked with at least the following information:
- Manufacturer's/Supplier's Name
- Brand Name
- Description
- Date of Manufacture
8.2 Operational Test Sample
Operational test samples shall consist of sufficient amount of catalyst that shall be
forwarded to the purchaser for operational test. Samples shall be plainly identified by
attached durable tag marked with at least the following information:
- Manufacturer's/Supplier's Name
- Brand Name
- Description
- Instruction for Use
- Analytical Control
- Dosage (with reference to Annex C)
- Storaging
- Date of Manufacture
9. INSPECTION
The manufacturer/supplier shall be responsible for carrying out all the tests required
by this standard specification, using his own or other reliable facilities, and he shall
maintain complete records of all such tests and qualifications. Such records shall be
available for review by the purchaser. The manufacturer/supplier shall furnish to the
purchaser a certificate of quality stating that each batch has been sampled, tested,
and qualified in accordance with this standard specification and has been found to
meet the requirements specified.
The manufacturer/supplier shall afford the purchaser’s inspector all reasonable
facilities required for inspection of each batch of production in accordance with this
standard specification. Such inspection in no way relieves the manufacturer/supplier
of his responsibilities under the term of this standard specification.
The purchaser reserves the right to perform any inspections set forth in this standard
specification where such inspections are deemed necessary to assure that supplies
and services conform to the prescribed requirements.
The purchaser’s inspector reserve the right to have access to the materials subject to
inspection for the purpose of witnessing selection of the samples, preparation of the
test samples and performance of the test(s). For such tests, the inspector reserves
the right to indicate the sample(s) from which the quantities will be taken in
accordance with the provisions of this standard specification.
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IGS-R-CH-052(0)
10. MARKING
10.1 Marking of Containers
Each container shall be legibly marked with at least following information:
Composition
MESC No.
Handling Guidelines
Safety Precautions
Storage Conditions
Date of Manufacture
Date of expiry
Batch No.
Order No.
Net weight
Gross weight
Name and Address of Manufacturer/Supplier
HMIS (Hazardous Material Identification System including health, fire, reactivity,
personal protection, specified hazard, etc)
10.2 Precautionary Marking
All individual containers shall be marked with precautionary symbols and/or phrases.
11. PACKAGING
11.1 The catalyst shall be suitably packed in approved containers in accordance with
the requirement of the purchase order.
11.2 The containers shall be protected against all damages or defects which may
occur during handling.
12. STORAGE LIFE
The catalyst shall meet all requirements of this standard specification at least 24
months from date of delivery at manufacturer's/supplier's mentioned storage
condition.
13. DOCUMENTATION
The manufacturer/supplier shall provide sufficient information and shall supply the
technical information as a minimum requirement as follows:
- ISO 9001 for management quality control of offered mercaptan oxidation catalyst
that be used for removing mercaptans from natural gas, LPG, butane and propane
issued by an internationally recognized body.
- Approval test report, original technical catalogues, manufacturing product data
sheet and application procedure recommendation and guidelines.
- Material Safety Data Sheet (MSDS).
- Filled, signed and stamped data sheet stating in Annex B.
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June 2012
IGS-R-CH-052(0)
"ANNEX A"
Mercaptan Oxidation Catalyst Typical Properties
Table A-1 provides typical properties for catalyst specified in this standard
specification and have been used in natural gas refineries.
Table A-1
Item
Characteristic
Unit
Value
Test Method
1
Chemical formula
---
Sulfonated Cobalt
Phthalocyanine
IR
2
Appearance
---
suspended liquid, dark
blue color, without smell or
sometimes a little
ammonia smell
Visual
3
Cobalt content
wt %
>5
Annex F
clause F.1
4
Solid content
wt %
>15
Adjustable
5
Ash percent of solid
content
wt %
<15
Annex F
clause F.2
6
Water content
wt %
<85
Adjustable
7
Density
g/cm3
1.05 – 1.2
Routine Procedure
8
pH
---
5–8
Routine Procedure
9
UV absorbance at λ max
---
≥3 at 667 nm
Annex F
clause F.3
10
Reduction of mercaptan
in condensate
ppm
<50
Annex F
clause F.4
11
Reduction of mercaptan
in naphtha and LPG
ppm
<8
Annex F
clause F.4
in liquid phase
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June 2012
IGS-R-CH-052(0)
"ANNEX B"
Catalyst Data Sheet
The following Tables shall be filled, signed and stamped by manufacturer/supplier.
Product designation
Manufacturer's/Supplier's name
Manufacturer's/Supplier's address
Table B-1
Item
Characteristic
1
Chemical formula
2
Appearance
3
Co content
4
Solid content
5
Ash percent of solid
content
6
Water content
7
Density
8
pH
9
UV absorbance at  max
10
Reduction of mercaptan in
condensate
11
Reduction of mercaptan in
naphtha and LPG
Unit
Value
Test Method
Remark
Notes:
1. This data sheet shall be filled, signed, and stamped by manufacturer/supplier.
2. Any deviation from this standard specification shall clearly be specified by
manufacturer/supplier at following table.
DEVIATION(S)
AUTORIZED SIGNATURE
COMPANY'S STAMP
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June 2012
IGS-R-CH-052(0)
"ANNEX C"
Mercaptan Removal Unit Data
The following Tables shall be filled by user.
1. Feed Gas/Liquid Composition:
Characteristic
N2
C1
C2
C3
iC4
nC4
iC5
nC5
C6
C7
C8
C9
C10+
H2S
Total sulfur
CO2
Total RSH
C1SH
C2SH
iC3SH
sec C4SH
Unit
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol ppm
mol ppm
mol ppm
mol ppm
mol ppm
mol ppm
mol ppm
mol ppm
Value
Unit
bar gauge
0
C
Value
Unit
ppm
ppm
Value
2. Inlet Gas/Liquid Condition:
Characteristic
Pressure
Temperature
3. Outlet Gas/Liquid Specification:
Characteristic
Mercaptan
Total sulfur
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IGS-R-CH-052(0)
"ANNEX D"
Gas Treating Plant Data
(Informative)
The following Tables could be filled by user and manufacturer/supplier for mercaptan
oxidation catalyst evaluation for field test approval.
1. EXTRACTION UNIT
1.1 Operational Report
1.1.1 Flow rate, per hour
Characteristic
Feed gas
Fresh prewash caustic
Caustic to gas line
Recycle caustic to prewash section
Recycle plus spillback
Lean caustic to prewash section
Fresh water
Circulating water
Lean caustic to extraction section
Unit
MMSm3
m3
m3
m3
m3
m3
m3
m3
m3
Value
1.1.2 Pressure, bar gauge
Characteristic
Value
Feed gas
Product gas
Prewash caustic break tank
Recycle pump discharge
Interface pot
Lean caustic break tank
Lean caustic pump discharge
Circulating water pump discharge
1.1.3 Temperature, 0C:
Characteristic
Value
Feed gas
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June 2012
IGS-R-CH-052(0)
1.1.4 Calculated data:
Characteristic
Lean caustic (prewash section)/feed
gas ratio
Carbonate content
Unit
---
Value
wt% spent caustic
1.2 Analyses Report
1.2.1 Feed gas composition:
Characteristic
Unit
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol %
mol ppm
mol ppm
mol ppm
mol ppm
mol ppm
mol ppm
mol ppm
mol ppm
N2
C1
C2
C3
iC4
nC4
iC5
nC5
C6
C7
C8
C9
C10+
H2S
Total sulfur
CO2
Total RSH
C1SH
C2SH
iC3SH
sec C4SH
Value
1.2.2 Prewashed gas composition, mol ppm:
Characteristic
Value
CO2
1.2.3 Treated product gas composition, mol ppm:
Characteristic
CO2
H2S
Total sulfur
Total RSH
Value
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IGS-R-CH-052(0)
1.2.4 Calculated feed gas composition data:
Characteristic
Molecular weight
Water content
Unit
--mol %
Value
1.2.5 Other calculated data, kg/h:
Characteristic
Mercaptan-sulfur extracted
Disulfide-sulfur reentered
Value
1.2.6 Prewash stage effluent caustic:
Characteristic
Specific gravity
Total alkalinity
Strong base
Mercaptide
Sulfide
Unit
--wt% NaOH
wt% NaOH
wt% Sulfur
wt% Sulfur
Value
1.2.7 Extraction stage rich caustic, wt ppm sulfur:
Characteristic
Mercaptide
Sulfide
Value
1.2.8 Water-wash stage effluent water
Characteristic
Value
pH
2. REGENERATION SECTION
2.1 Operational Report
2.1.1 Flow rate, per hour:
Characteristic
Unit
Sm3
Sm3
m3
m3
Total air
Mixed gas to burner
Catalyst solution
Lean caustic
10
Value
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June 2012
IGS-R-CH-052(0)
2.1.2 Pressure, bar gauge:
Characteristic
Catalyst pump discharge
Rich caustic surge drum
Oxidiser inlet
Oxidiser outlet
Air separator
Value
2.1.3 Temperature, 0C:
Characteristic
Oxidiser inlet
Oxidiser outlet
Value
2.1.4 Calculated data:
Characteristic
Number of contactor(s) at service
Total sulfur load
Theoretical air need
Excess air used
Total gas treated
Catalyst used
Total fresh caustic
Caustic soda used
Total caustic to contactor
Caustic to oxidiser
Unit
--kg/h
Sm3/h
volume %
Sm3/h
kg/MMSm3
m3/h
kg/MMSm3
m3/h
m3/h
Value
Unit
--wt% NaOH
wt% NaOH
wt ppm Sulfur
wt ppm Sulfur
wt ppm Sulfur
wt ppm
Value
2.2 Laboratory Analyses
2.2.1 Lean caustic, regenerated:
Characteristic
Specific gravity
Total base
Strong base
Mercaptide
Sulfide
Thiosulfate
Extractible-sulfur
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IGS-R-CH-052(0)
2.2.2 Mixed caustic to oxidiser, wt ppm sulfur:
Characteristic
Mercaptide
Sulfide
Value
2.2.3 Spent air system, volume %:
Characteristic
Vented air, O2 content
Air + Fuel gas blend, O2
Value
2.2.4 Field test, second:
Characteristic
Lean caustic shake test
Value
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IGS-R-CH-052(0)
"ANNEX E"
Propane/Butane/LPG Treating Plant Data
(Informative)
The following Tables could be filled by user and manufacturer/supplier for mercaptan
oxidation catalyst evaluation for field test approval.
1. EXTRACTION UNIT
1.1 Operational Report
1.1.1 Flow rate, m3 per hour
Characteristic
Liquid(C3,C4,LPG) flow rate
Caustic flow rate
Water circulation
Value
1.1.2 Pressure, bar gauge
Characteristic
Propane /Butane/LPG
Caustic
Value
1.1.3 Temperature, 0C:
Characteristic
Propane /Butane/LPG
Caustic
Value
1.2 Finishing Drum Stage Effluent Caustic:
Characteristic
Specific gravity
Concentration
Na2S
Mercaptide
Unit
--wt% NaOH
mg/kg
wt% Sulfur
13
Value
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June 2012
IGS-R-CH-052(0)
1.3 Feed Liquid Composition:
Characteristic
Unit
vol %
vol %
vol %
vol %
vol %
vol %
vol %
mg/kg
--psig
C1
C2
C3
iC4
nC4
iC5
nC5
Total sulfur
Specific gravity at 60 0F
R vapor pressure at 100 0F
Value
1.4 Prewashed Gas Composition, mol ppm:
Characteristic
Value
CO2
1.5 Treated Product Liquid Specification, mol ppm:
Characteristic
Total sulfur
Total RSH
Value
1.6 Water-Wash Stage Effluent Water
Characteristic
Value
pH
2. REGENERATION SECTION
2.1 Operational Report
2.1.1 Flow rate, per hour:
Characteristic
Process air
Total air
Catalyst solution
Lean caustic to
propane/Butane/LPG extractor
C4 injected flow rate for washing
Unit
kg
kg
ppm
m3
m3
14
Value
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June 2012
IGS-R-CH-052(0)
2.1.2 Pressure, bar gauge:
Characteristic
Catalyst drum
C4 washing drum
Oxidiser inlet
Oxidiser outlet
DSO separator
Value
2.1.3 Temperature, 0C:
Characteristic
Oxidiser inlet
Oxidiser outlet
Value
2.1.4 Calculated data:
Characteristic
Total sulfur load
Total gas treated
Catalyst used
Total fresh caustic every week
Caustic soda used
Total caustic to contactor
Caustic to oxidiser
Unit
kg/h
m3/h
liter
m3
kg/MMSm3
m3/h
m3/h
Value
Unit
--wt% NaOH
g/l
g/l
wt ppm Sulfur
wt ppm Sulfur
wt ppm Sulfur
Value
2.2 Laboratory Analyses
2.2.1 Lean caustic, regenerated:
Characteristic
Specific gravity
Concentration
Total alkalinity
Free alkalinity
Mercaptide
Sulfide
Thiosulfate
2.2.2 Spent air system, volume %:
Characteristic
Vented air, O2 content
Value
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June 2012
IGS-R-CH-052(0)
"ANNEX F"
Test Methods
This Annex contains the test methods referenced in Annex A.
F.1 Cobalt Content Test Procedure by Atomic Absorption
-. Weight 0.2 gr sample with accurately 0.1 mgr at 100 mlit beaker;
-. Add drop by drop 20 ml of 0.65 nitric acid while stirring;
-. Cover the beaker with watch glasses and heat on electric heater up to 80 0C for
one hour slowly;
-. Transfer the sample to 100 ml flask by deionized water and then dilute;
-. Calibrate atomic absorption apparatus with standard sample and then measure the
solution concentration.
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IGS-R-CH-052(0)
F.2 Ash Content Measurement Test Procedure
This procedure is done in two steps:
F.2.1 Drying of the Sample
-. Weight 0.2 gr sample inside porcelain;
-. Keep the sample at 150 0C for 3 hour and then place it in desiccator until reaches
to room temperature;
-. Reweight the sample and measured the dried sample.
F.2.2 Ash Content Measurement
-. Heat the dried sample of previous step up 650 0C for 3 – 16 hour and then place
the sample in desiccator until reaches to room temperature;
-. Weight the sample and then calculate ash content by divide quantity of heated
sample to dried sample and multiple 100.
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IGS-R-CH-052(0)
F.3 UV/Visible Spectroscopy Absorption Measurement Test Procedure
In case, the catalyst is liquid:
-. Dilute 0.15 ml of 30% mass percent catalyst solution to 1000 ml by deionized
water;
-. Measure the amount of absorption with spectroscope.
In case, the catalyst is in powder form:
-. Weight 5 mgr catalyst and then add it to 80 ml deionized water;
-. Add 1-2 drops of 3 normal sodium hydroxide solution to it;
-. After homogenization, add 1 drop of 25% ammonia;
-. Measure the amount of absorption quantity with spectroscope.
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F.4 Test Procedure for Determining Activity of Demercaptanization
Catalyst in Gas Condensate
F.4.1 Determination of Condensate Sulfur Content
-. Determine H2S content;
Note: Up to 100 ppm, step F.4.2 and F.4.3 and less than 100 ppm only step F.4.3 should be
done;
-. Determine RSH content;
-. Determine total sulfur content.
F.4.2 Condensate Wash with 25% Diethanolamine Aqueous Solution
-. Pour condensate and diethanolamin solution (25%) with 2 to 5 volumetric ratios in
a three neck flask.
The flask should be equipped with water bath, temperature controller, mechanical
mixer, thermometer and condenser. This condition shall be kept at 40 - 45 0C for 30
minutes.
-. Transfer flask content to the decanter, then separate hydrocarbon cut and aqueous
cut and weight each one accurately and keep them at sample vessels;
-. Determine H2S, RSH and total sulfur content in hydrocarbon cut;
-. Determine total sulfur content in aqueous cut.
F.4.3 Washing Hydrocarbon Cut of Step F.4.2 with Sodium Hydroxide 15%
Solution
-. Pour hydrocarbon cut of step F.4.2 with sodium hydroxide (15%) with 2 to 5
solution volumetric ratios in a three neck flask.
The flask should be equipped with water bath, temperature controller, mechanical
mixer, thermometer and condenser. This condition shall be kept at 50 0C for 30
minutes.
-. Transfer flask content to the decanter then separate hydrocarbon cut and aqueous
cut and weight each one accurately and keep them at sample vessels;
-. Determine H2S, RSH and total sulfur content in hydrocarbon cut;
-. Determine total sulfur content in aqueous cut.
F.4.4 Sodium Mercaptide Reaction with Catalyst at Aqueous Cut of Step F.4.3
-. Keep catalyst and aqueous cut solution mixture with 1 to 10 volumetric ratios in
autoclave for reaction at following condition:
-. Residence time: 160 minutes (depend on mercaptan condensate content);
-. Temperature: 60 0C;
-. Pressure: 4 - 5 barg;
-. Air content: 10 Nl/h;
-. Catalyst solution concentration: 2000 ppm.
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F.4.5 Extraction of Step F.4.4 Product Reaction with Desulfurized Naphtha
(Catalyst Reforming Unit Feed)
-. Determine H2S, RSH and total sulfur at naphtha cut;
-. Extraction reaction should be done in autoclave at two different pressures by
following condition:
-. Naphtha cut to aqueous cut ratio: equal to 1 to 20;
-. Residence time: 3 hour;
-. Temperature: 60 0C;
-. First step extraction pressure is 3 barg and second step extraction pressure is 2
barg (extraction could be done in flask system at atmospheric pressure);
-. Determine total sulfur content in aqueous and naphtha cuts.
F.4.6 Reaction of Sodium Mercaptide with Catalyst at Step F.4.3 Hydrocarbon
Cut
-. Reaction should be done in three neck flask equipped with water bath, temperature
controller, mechanical mixer, thermometer and condenser by following condition:
-. Catalyst solution to hydrocarbon cut ratio is equal 1 to 10;
-. Alkaline catalyst solution concentration should be 2000 ppm and %2 sodium
hydroxide
-. Temperature is 50 0C;
-. Valid sampling time is from 2 minutes to 120 minutes,
-. Determine RSH and total sulfur in samples and then resolve catalyst conversion
quantity.
20