Spec.

: 1E55-40-600
SULPHUEX PLANT
Rev.: 0

JOB: 1E55 Sheet: 1 of 119

ARMA SOAP & DETERGENTS

EGYPT

OPERATION HANDBOOK

JOB 1E55

0 First Issue July 2011 MSP

Rev. Descrizione / Description Data / Date Autore / Author
The master version of this document is stored as a digital file in a software archive - Approval process is digitally managed, details do not
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1E55-40-600 Operation Handbook 2

Table of contents
1. Drawing list............................................................................................................... 5
1.1 Plant basis of design ...................................................................................................... 5
1.2 Plant capacity.................................................................................................................. 6
1.3 Raw material specification ............................................................................................. 6
1.4 Utilities specification ...................................................................................................... 9
1.5 Product quality .............................................................................................................. 10
1.6 Site condition ................................................................................................................ 11
2. Process description ............................................................................................... 12
2.1 Introduction ................................................................................................................... 12
2.2 Air drying ....................................................................................................................... 12
2.3 Sulphur melting and proportioning ............................................................................. 13
2.4 SO2 / SO3 production .................................................................................................... 13
2.5 Film sulphonation / sulphation .................................................................................... 14
2.6 Ageing / Stabilizing ....................................................................................................... 15
2.7 Exhaust gas treatment ................................................................................................. 15
2.8 Double step neutralisation ........................................................................................... 15
2.9 SLES deareation unit .................................................................................................... 16
3. R.M. handling & recommended safety equipment .............................................. 17
3.1 R.M. handling ................................................................................................................ 17
3.2 Recommended safety equipment ................................................................................ 19
4. Safety prescriptions .............................................................................................. 20
4.1 Introduction ................................................................................................................... 20
4.2 General prescriptions ................................................................................................... 20
4.3 Typical risks .................................................................................................................. 21
4.3.1 EYE CONSERVATION ......................................................................................................................21
4.3.2 NOISE EXPOSURE AND HEARING CONSERVATION ..............................................................................21
4.3.3 CHEMICAL RISK .............................................................................................................................21
4.3.4 ELECTRICAL RISK ..........................................................................................................................22
4.3.5 MAINTENANCE ACTIVITIES ON EQUIPMENTS ......................................................................................22
4.3.6 LOAD HANDLING ............................................................................................................................23
4.3.7 OBJECT OR MATERIALS FALL ..........................................................................................................23
4.3.8 HEAD HITS, FALL, SLIDING AND STUMBLING .......................................................................................24
4.3.9 BURNS.........................................................................................................................................24
4.3.10 VESSELS AND CONFINED SPACES ..................................................................................................25
4.3.11 PERSONAL PROTECTIVE EQUIPMENTS ...........................................................................................25
5. Pre-commissioning ................................................................................................ 28
5.1 Check list for plant completion .................................................................................... 28
5.2 Pressure test ................................................................................................................. 28
5.3 Mechanical procedures ................................................................................................ 34
5.4 Electrical procedures ................................................................................................... 39
5.5 Computer procedures .................................................................................................. 41
1E55-40-600 Operation Handbook 3

5.6 Special equipment procedures .................................................................................... 42

5.7 Pre-commissioning completion .................................................................................. 44
5.8 Pre-commissioning procedures: WHAT IF .................................................................. 45
5.9 Pre-commissioning procedures: HAZARD IDENTIFICATION .................................... 68
6. Commissioning and start-up procedure .............................................................. 83
6.1 Procedures before plant start up ................................................................................. 83
6.2 Utilities start up ............................................................................................................. 84
6.3 Raw material circulation start up ................................................................................. 84
6.4 Refrigeration group start up......................................................................................... 85
6.5 Exhaust gas treatment start up.................................................................................... 85
6.6 Air drying section start up ........................................................................................... 86
6.6.1 SILICA GEL REEGNERATION PROCEDURE .........................................................................................87
6.7 Pre-heating burner start up .......................................................................................... 89
6.8 Sulphur melting and dosing pump setting / start up .................................................. 90
6.9 Electrical igniter 12H3 start up..................................................................................... 90
6.10 SO3 production start up ........................................................................................... 91
6.11 Sulphonic acid production start up ......................................................................... 93
6.11.1 RAW MATERIALS/PRODUCT ROUTING ............................................................................................93
6.11.2 SULPHONATION START UP SEQUENCE ...........................................................................................93
6.11.3 AGEING STABILIZING UNIT START-UP .............................................................................................94
6.12 Double step neutralization start up / shut down .................................................... 95
6.13 SLES deareation unit start-up .................................................................................. 96
6.14 Commissioning and start-up procedures: WHAT IF ............................................... 97
6.15 Commissioning and start-up procedures: HAZARD IDENTIFICATION................ 100
7. Steady running condition .................................................................................... 104
7.1 Oleum circuit ................................................................................................................... 104
7.2 Operating log sheet ........................................................................................................ 104
7.3 Analysis .......................................................................................................................... 104
7.4 Reports............................................................................................................................ 104
7.5 Pressure drops ................................................................................................................ 105
7.6 Off-spec recovery ............................................................................................................ 105
7.7 E.S.P. purging sequence................................................................................................. 105
8. Plant shut down ................................................................................................... 106
8.1 Raw material change over and capacity variation ........................................................ 107
10. Emergency shut down ......................................................................................... 110
10.1 Introduction ............................................................................................................. 110
10.2 Raw material feeding failure to 16R1 ..................................................................... 110
10.3 Air blower 11K1 troubles ........................................................................................ 110
10.4 Power failure ............................................................................................................ 110
1E55-40-600 Operation Handbook 4

11. Troubleshooting ................................................................................................... 111

12. Annexes ................................................................................................................ 119
1E55-40-600 Operation Handbook 5

1. Drawing list
Dwg. 1E55.10.002 - Sect. 11
Dwg. 1E55.10.003 - Sect. 12
Dwg. 1E55.10.004 - Sect. 14
Dwg. 1E55.10.005 Sheet 1&2 - Sect. 16
Dwg. 1E55.10.006 - Sect. 17-22
Dwg. 1E55.10.007 - Sect. 25
Dwg. 1E55.10.008 - Sect. 28
Dwg. 1E55.10.009 - Sect. 07

1.1 Plant basis of design

The film sulph(on)ation plant is based on Ballestra SULPHUREX continuous process to sulphonate
in a multitube film reactor, using SO 3 in variable quantity and concentration as sulphonation gas, all
the raw materials in the field of detergents and cosmetics, such as dodecylbenzene, linear
alkylbenzene, natural synthetic alcohols, ethoxylate alcohols, alpha-olefins, methyiesters,etc.
The project concerns a sulphonation plant, based on Ballestra’s SULPHUREX/F continuous
process, designed to produce sulphonic acid and active matter from all the main raw materials
used in the detergent industry.
Plant configuration consists of the following units:

 Air drying (sect. 11, DWG 1E55.10.002)

 Sulphur melting and proportioning (sect. 25, DWG 1E55.10.007)
 SO2 / SO3 production (sect. 12, DWG 1E55.10.003)
 Film sulphonation / sulphation (sect. 16, DWG 1E55.10.005 sh. 1 of sh. 2)
 Ageing / stabilizing (sect. 16, DWG 1E55.10.005 sh. 2 of sh. 2)
 Exhaust gas treatment (sect. 14, DWG 1E55.10.004)
 Double step neutralisation (sect. 17-22, DWG 1E55.10.006)
 SLES paste deareation (sect. 28, DWG 1E55.10.008)
 Finishing Unit (sect. 07, DWG 1E55.10.009)

The Plant can be easily stopped and started, so that a weekly operation is usually performed.
The plant operates continuously on daily shifts.
1E55-40-600 Operation Handbook 6

1.2 Plant capacity

The plant will perform as indicated hereinafter, provided that:
 the operation and maintenance activity are in compliance with the instructions given in the
plant manuals;
 the operating personnel is trained and capable;
 the raw materials and utilities are as for the characteristics here indicated.

SO3 production
The SO3 production is sized for up to 300 kg/h of sulphur with an operating range of 60 to 100%

Film sulphonation/Neutralization
The sulphonation/neutralization unit has the following capacity, in accordance to different
feedstocks

Ex Raw Material Capacity (100% AM as sodium salt)

- LAB m.w. 245 3000 kg/h

- Lauryl alcohol m.w. 207 2700 kg/h

- C16 – C18 alcohol m.w. 258 2700 kg/h

- Lauryl ether 2EO m.w. 283 1950 kg/h

- Lauryl ether 3EO m.w. 339 2220 kg/h

1.3 Raw material specification

Raw materials having the following shown characteristics are supposed to be made available at
battery limits.

Organic Raw materials

The product characteristics listed in section 5 are related to the used of high quality, international
standard, detergent grade raw materials as supplied by SHELL, CONDEA, PETRESA, HENKEL,
etc. and having main characteristics as listed here below
1E55-40-600 Operation Handbook 7

Linear DDB

Molecular weight : 235  245

Bromine number (gr. Br2/100 g) : 0.010 max
Color saybolt : 29 min
Water content : 0.01% max
Iron content : 1 ppm max. as Fe
Chain length distribution : Less than C10 1% max
C10 10  20%
C10C11 40  60%
C12 Min. 25%
C13 5  20%
More than C13 1  10%
2- phenil isomers 15  30%
Paraffins : 0.2 wt %
Alkyltetralins : 0.2 wt %
Normal alkylbenzene : 95 wt %
Specific gravity (at 15°C) : 0.856  0.865

Branched DDB

Molecular weight : 235-250

Bromine number : 0.05 max.
Water content : 0.05% max.
Iron content : 1 ppm max. as Fe

Lauryl alcohol
Molecular weight : 193-208
Iodine number (gr. J2/100 g) : 0.1 max.
Water content : 0.05% max.
Iron content : 1 ppm max. as Fe
Hydroxyl number (mg KOH/g) : 270-290
Chain length distribution C10 0-2 %
C12 50-75%
C14 25-40%
More than C14 0-2 %
1E55-40-600 Operation Handbook 8

Lauryl alcohol + 2EO/3EO 2EO 3EO

Molecular weight : 275-286 330  340

Water content (%) : 0.1% max. 0.1% max
(recommended) : 0.05% max. 0.05% max.
Iron content (as ppm Fe) : 1 max. 1 max
Polyglycol content : 0.5% max. 0.5% max
Hydroxyl number (mg KOH/g) : 196-204 165  170

Fatty alcohol C16-C18

Molecular weight : 255-274

Iodine number (gr. J2/100 g) : 0.5 max.
Water content : 0.05% max.
Iron content (as ppm Fe) : 1 max.
Hydroxyl number (mg KOH/g) : 205-220
Chain length distribution : C14 0-2 %
C16 40-50%
C18 40-50%
C20 0-3 %

Chemical Raw Materials

Sulphur
Purity : 99.7% min.
Ashes : 0.05% max.
Water content : 0.01% max.
Bitumen content : 0.02% max.
Acidity (as H2SO4) : 0.01% max.
Arsenic content : 2 ppm max.
Selenium content : 2 ppm max.
Tellurium content : 2 ppm max.
Physical state : Solid or liquid

Caustic soda solution

Concentration : constant as possible in the range 30-50%
Iron content : 5ppm max as Fe on 100% NaOH
Chloride content : 2% max as NaCl
Carbonate content : 1% max as Na2CO3
1E55-40-600 Operation Handbook 9

Phosphoric acid solution

Concentration : 85% wt
Pressure (at elevation 0 mt) : atmospheric (to be charged manually to buffer
tank)

1.4 Utilities specification

Utilities and chemicals having these characteristics are supposed to be made available at battery
limits.

Process water
Type: clean and filtered
Pressure min: 2 bar g
Pressure max: 4 bar g
Pressure operating: 3 bar g
Temperature: Ambient
Hardness: 20°F max

Cooling water
Pressure supply min: 4 bar g
Pressure supply max: 6 bar g
Pressure supply operating: 5 bar g
Pressure return: atmospheric at 8 mt. elevation
Temperature In: 30°C max

Hot water
Pressure In: 2 bar g min.
Temperature In: 70°C

Steam
Type: saturated
Pressure in max: 12 bar g
Pressure in min: 9 bar g
Pressure operating: 10 bar g

Fuel
Type: Natural gas
Pressure: 4 bar g
Low heat value: 8500 Kcal/Nm3

Instrument air
Type: dried and oil free
Pressure in max: 6 bar g
Pressure in min: 4 bar g
Pressure operating: 5 bar g
Dew point: -20°C

Electric power
Driving power: 380 V , 50 Hz, 3 phases
Tropicalization: Yes
1E55-40-600 Operation Handbook 10

1.5 Product quality

Using raw materials of high quality as specified in para 4, the product obtained will have the
following characteristics:

Raw Materials A.M. % free oil % sulphate °Klett

conc. % * * **

A Linear DDB:
as neutralised paste (1) 60 1 1.5 25
as sulphonic acid 97 1.07 1.1 *** 25

B Natural Lauryl Alcohol (1)

C12-C14 or C12-C18 30 1.5 1.5 10

C Synthetic alcohol C12-C14 (1)

(type Alfol, Ethyl, Dobanol 25) 30 1.5 1.5 10

D Natural alcohol (type Dehydol LS2)

or synthetic (type Dobanol 25/2) 27 1.5 1.5 20
ethoxylated with 2EO (1) 70

E Same as above, but ethoxylated

with 3EO 27 1.5 1.5 20
(type Dehydol LS3/Dobanol 25/3) 70
(1)

* On 100% Active Matter as sodium salt

** 5% A.M. solution, 40 mm cell N° 42 filter, unbleached, unless otherwise specified.
*** As 100% H2SO4
(1) With the installation of neutralisation

Notes: The free oil guaranteed figures are achievable when the r.m. sulph(on)ability is 99% min.
In case of different sulph(on)ability level (and in particular for DDB) the guaranteed free oil figure
will correspond to a 99.5% yield of the sulphonatable compounds:

Example (for DDB m.w. 245):

- Sulphonability (S) = 98.5%

- Sulphonation yield (Y) = 99.5%
- m.w. DDB/DDBS = 245/325

free oil on 100% = ( 100 – SY ) x m.w. DDB x 10000 =

sulphonic acid = 100 m.w. DDBS SY
( 100 – 98.5 x 99.5 ) x 245 x 10000 = 1.533
100 325 98.5 x 99.5
1E55-40-600 Operation Handbook 11

Dioxane guarantee on sodium lauryl ether sulphate (SLES)

As a complement of product quality figures herein above listed and with special reference to the
1.4-DIOXANE ISSUE, Ballestra is ready to guarantee a maximum content of 50 ppm (30 ppm
expected for a wide range of raw materials) of 1.4-DIOXANE in SLES at the following conditions:

- Operation with SO3 gas at 2,75% volume concentration (already foreseen in base plant
configuration);

- Top quality raw materials processing such as ethoxylated alcohol coming from natural C12-
C14 alcohols (Henkel LOROL), Ziegler alcohols (ALFOL) or oxo-alcohols (DOBANOL serie)
having the characteristics previously listed and:

 Ethoxylation degree : 3EO max.

 Moisture content : 0,05% max

- Free oil in 100% Active Matter:

 2% for SLES - 2EO

 2.5% for SLES - 3EO

If the characteristics of the raw materials before ethoxylation or the ethoxylated alcohol are
different from the listed figures, and/or one or more of the specified process conditions are
different, the guaranteed 1.4-DIOXANE content will be defined case by case.

1.6 Site condition

The design and the selection of the plant equipment/materials will be made according to the
following site conditions:

Climatic conditions

 Design wet bulb temperature : 30°C

 Design dry bulb temperature : 40°C
 Air temperature (min / max) : 10°C / 40°C
 Relative humidity design : 65% at 35°C (Equivalent to 25 gr H2O/kg dry air)

Geographic/geophysics data

 Height above sea level : mt. 110

 Max wind speed : 33 m/sec
 Seismic degree (M.M.S. - ANSI 58.1) : Zone 2
1E55-40-600 Operation Handbook 12

2. Process description

2.1 Introduction
The project concerns a sulphonation plant, based on Ballestra’s SULPHUREX/F continuous
process, designed to produce sulphonic acid and active matter from all the main raw materials
used in the detergent industry.

Plant configuration consists of the following units:

 Air drying (sect. 11, DWG 1E55.10.002)

 SO2 / SO3 production (sect. 12, DWG 1E55.10.003)
 Exhaust gas treatment (sect. 14, DWG 1E55.10.004)
 Film sulphonation / sulphation (sect. 16, DWG 1E55.10.005 sh. 1 of sh. 2)
 Ageing / stabilising (sect. 16, DWG 1E41.10.005 sh. 2 of sh. 2)
 Double step neutralisation (sect. 17 / 22, DWG 1E55.10.006)
 Sulphur storage and proportioning (sect. 25, DWG 1E55.10.007)
 SLES deareation unit (sect. 28, DWG 1E55.10.008)

2.2 Air drying

Air required for sulphur combustion and SO 2 / SO3 production is filtered and compressed by low
pressure blower 11K1.
In order to remove the compression heat and to condense the major part of the moisture, air is
indirectly cooled in 11E3 by cooling water first, and then in 11E4 by glycol solution (coming from
the chilling group 11RG1).
The process air, at approx. 5°C, is then conveyed to the silica gel dryer (11C1).
The silica gel dryer is composed of two separate units working in parallel; when one unit is "on line"
(absorbing water from the air) the other is kept under regeneration.
Each unit is designed to achieve a dew point of –70°C. Dew point of process air is detected by a
on-line dew-point meter.
The silica gel dryers work in parallel; when one unit is on operation (absorbing water from the air)
the other one is kept under regeneration.
The silica gel regeneration is made by hot air circulation, in order to evaporate all the water
absorbed; hot air employed in the regeneration comes from SO 2/SO3 coolers (12E2, 12E3, 12E5).
This stream is typically at a temperature of about 300-350°C, therefore further heating by means of
steam in regeneration battery (11E1) is not required, and as a matter of fact a dilution with
atmospheric cold air is preferable to perform the regeneration at a temperature of about
160÷170°C.
When regeneration is complete, it is necessary to cool down the bed before feeding the process air
to be dehumidified. The cooling operation is performed by passing cold air through the bed, taking
care of not to bring moisture in and therefore decrease the adsorptive capacity of the bed before
starting a new drying cycle. Cold air is obtained recycling air in a close loop through the bed and
the regeneration battery (11E1), having cooling water flowing inside the coils. Switching from water
absorption to regeneration is performed automatically by means of remote controlled ON/OFF
valves driven by a dedicated logic.
1E55-40-600 Operation Handbook 13

2.3 Sulphur melting and proportioning

The solid sulphur is melted and filtered to avoid the pump clogging and then fed to the sulphur
burner by an immersed pump (25P1)
A second pump 25P2 is supplied as stand-by .
The mass flow rate of sulphur pumped to the furnace is controlled by a mass flow meter FE/ FT
25.1; an automatic P.I.D. control loop constantly adjusts the rotation speed of the pump motor in
order to keep the sulphur flow rate at the wished value.
In order to avoid pump valves clogging, molten sulphur is filtered by filters 25F1/F2 located
upstream the melting vessel portion where the immersed gear pumps are installed.
Pumps and relevant piping are heated with saturated steam - 4 Bar (g) - in order to keep the
sulphur temperature at 140-150°C.
In this way the viscosity, and therefore the pressure drops, are kept as low as possible.

2.4 SO2 / SO3 production

Molten sulphur is fed by pumps 25P1/25P2 to the burner 12H1 counter-currently to the combustion
air, and falls on a layer of refractory balls.
The unit is started by electric igniter 12H3, but as the sulphur burns, being the combustion “self
sustaining”, the igniter is turned off.
The design of the unit is very simple and allows complete sulphur combustion without any spraying
nozzle that might often get clogged due to sulphur impurities.
The reaction taking place in the burner is:

S + O2  SO2
(Sulphur) (Oxygen) (Sulphur dioxide)

SO2 comes out from the burner at around 650°C at a concentration of approx. 7% by volume.
The gas is then cooled to about 435°C by the heat exchanger 12E2 located on the top of SO 2/SO3
conversion tower 12C1.
Inside the conversion tower, four layers of catalyst (Vanadium) are present, and the reaction
temperature is kept at the optimum value by inter-stage cooler 12E3 and by quench air streams.
The conversion reaction is the following:

SO2 + 1/2 O2  SO3

(Sulphur dioxide) (Oxygen) (Sulphur trioxide)

The gaseous SO3 stream comes out from column 12C1 at about 430°C and is cooled down to
60°C by means of shell and tube heat exchangers 12E5 and 12E6.
Hot air coming from the SO2/SO3 converter coolers (12E2 and 12E3) and from SO 3 cooler 12E5 is
collected and sent to11C1 for regeneration when required.
During the plant start-up, a preheating system has been designed in order to warm up the
converter; the system is based on a hot air generator (12H2) and a burner (12H4) fed with natural
gas, generating an hot air stream at 580°C.
Hot air flows to the exchanger 12E2 (tube side) and heats the process air stream flowing inside the
tower to warm up the converter.
When the temperature measured at the outlet of the first catalyst bed will reach approx. 380°C and
all the other beds will be hot, it will be possible to start feeding sulphur to the furnace; in this way
the heat generated by sulphur combustion will warm up the converter until design conditions will be
reached.
1E55-40-600 Operation Handbook 14

2.5 Film sulphonation / sulphation

SO3 gas, coming from 12E6, is diluted with dry air at requested value for the specific feedstock and
diluted SO3 stream is filtered in brink-type filter 16F3.
The sulphonation gas is fed to the top of the reactor 16R1 and distributed exactly in equal parts
into each reaction tube.
The raw material coming from battery limit is filtered in 16F4 A/B and then fed to the reactor 16R1
in co-current with the gas.
A great advantage of the Ballestra’s film sulphonation plant is the special design of the reactor
distribution heads, which gives the possibility to dose accurately and to keep the exact mole ratio
between the raw material and the sulphonation gas in each single reaction tube, and to self-
equilibrate it, thus eliminating any risk of over-sulphonation.

The sulphonation reaction taking place in the reactor is:

R-H + SO3  R-SO3H

(LAB) (Sulphur trioxide) (Sulphonic acid)

The sulphation reaction taking place in the reactor is:

RO- CH2CH2-(CH2CH2O)n-OH +SO3  R-(CH2CH2O)n+1-OSO3H

(Ethoxylated alcohol) (Sulphur trioxide) (Sulphonic acid)

This feature is very important when sensible raw materials such as alcohols and ethoxylated
alcohols are processed or top quality LABS must be produced. The exact mole ratio between SO 3
and organic feedstock is essential to obtain the maximum conversion degree with optimum color.
In film reactors of different types, the equilibrium is achieved only by the utmost accuracy in the
mechanical construction; it is rather difficult to obtain such accuracy in large size plants and to
keep it unchanged during the life of the equipment (owing to assembly and disassembly, during
maintenance, caused by charring of the distribution area, which has a negative influence on the
homogeneity of the gas/liquid distribution), while the Ballestra reactor is self-equilibrating as
described before.
The heat of reaction is removed in the shell side by cooling water, automatically thermo-stated in
accordance with each raw material processed.
A further advantage of Ballestra’s film sulphonation plant consists in the emergency system, which,
in case of a sudden lack of raw material due for example to power failure, enters automatically in
operation, cutting off the SO3 flow and feeding fresh organic feedstock through the reactor thereby
avoiding any over-sulphonation of the product under processing and any need of cleaning the
reactor for charring due to lack of liquid; this liquid is recovered in an off-spec cubitainer from
where can be recycled to the reactor by means of pump 16P3 when the plant running is resumed.
The sulphonic acid coming out from the reactor 16R1 is degassed in the 16S2 and is sent, by
means of pump 16P2, to the ageing / stabilising unit or directly to the neutralisation unit (according
to the product handled).
The procedure for product change-over is very simple, as the product residence time in the
sulphonation system is very low.
This operation can be effected on line, simply by feeding the new raw material instead of the
previous one; to avoid any possibility of mixing the new products, the sulphonic acid can be
conveyed for few minutes maximum to the slop tank for recovery and collected in drums.

Sulphonation degree control XIC.16.1

Ballestra has developed and successfully tested a “Sulphonation degree control system”, based on
the use of mass flow meters indicating mass flow and density of the product under process.
1E55-40-600 Operation Handbook 15

When the XIC.16.1 is set in Automatic mode, the raw material control loop FIC.16.3 is reset on the
actual density DI.16.4 of the product outflowing the reactor, that is strictly related to the
sulphonation degree.
The operator, before to insert the Sulphonation degree control XIC.16.1 in auto mode, will check
the correct density value by analysis and compare it with the process density value DI.16.4.
When the acid value detected by analysis will be correct and the density value stable, the operator
will fix the detected density value as a set point and put the controller in auto mode.
The system is therefore independent also of eventual fluctuations of the SO 2/SO3 conversion yield.

2.6 Ageing / Stabilizing

When linear alkyl benzene (LAB) is used as raw material, sulphonic acid from 16P2 must be sent
to vessel 16A1 where is aged at controlled temperature to complete the sulphonation reaction.
Acid coming out from 16A1 is then stabilized adding water and finally cooled to about 40°C in the
plate heat exchanger 16E1, before being sent to battery limits.

2.7 Exhaust gas treatment

The exhaust gas stream coming from 16S1 is treated before being sent to the atmosphere, in order
to remove any possible organic, unreacted SO 3 traces and unconverted SO2.
The gas stream, containing traces of organic matter and partially sulphonated raw material, is sent
to the electrostatic precipitator 14F1 designed to ensure high organic/SO 3 mist separation. In this
unit, an high voltage difference is originated between the electrodes and the discharge pipes,
which charges of electricity the liquid impurities.
Being the impurities and pipes electric charge of opposite sign, the former are attracted to the
pipes walls. Here, they coalesce in form of liquid drops which fall down and are collected in the
bottom of the electrostatic precipitator.
The collected product is continuously discharged in an external drum.
In order to keep clean the insulating elements of the electrodes, a stream of air, at a temperature of
60°C. approx. is conveyed by the fan 12K1 to the ESP.
The gaseous stream coming from 14F1 and containing the unconverted SO2 is treated in the
packed scrubbing column 14C1, where water and caustic soda solution are continuously added
and recycled by pump 14P1.
The SO2 reacts with the caustic soda to obtain sodium sulphite, which is discharged as aqueous
solution; part of the sulphite is oxidised to sulphate in the column itself by the oxygen contained in
the exhaust gas.
The exhaust gas stream is saturated with water and sent to the atmosphere.
The caustic soda solution feeding is effected automatically in accordance with the sulphites
solution pH.

2.8 Double step neutralisation

The unit is designed to neutralise the sulphonic acid by means of caustic soda, fed from the battery
limits to the metering pump 17P1, through the intermediate storage tank 17V1.
The dilution water is also fed to plant via metering pump 17P1, through the intermediate storage
tank 17V2.
1E55-40-600 Operation Handbook 16

Metering pump 17P1 is fitted with 4 piston heads; two of them designed for process water dosing
and two heads for caustic soda dosing. The dilution water dosing is set manually by the operator
through the piston stroke of 17P1, in order to achieve the required paste concentration.

The pH in the neutralising unit is automatically controlled from the computer, by means of the pH-
meter AIC17.1 acting on the piston head “D” which is designed with a small flow capacity, in order
to finely tune the alkaline solution dosing. The main flow of caustic soda is set manually from the
operator through the piston stroke of head C.

The sulphonic acid coming from 16P2 or 16P4 (according to the raw material processed), the
process water and the caustic soda are continuously fed to the neutralising loop, consisting of
mixer 17MX1, circulation pump 17P2 and heat exchanger 17E1.

The most of the product is continuously recycled through the neutralising loop, whereas part of it is
continuously discharged to finishing tank, controlled by means of the pressure controller PIC17.3,
acting on pneumatic valve PV17.3.

Inside the neutralising loop the paste is maintained alkaline (free alkalinity is kept as low as 0.2%).

The paste outflowing the neutralising loop, passes through the second mixer 22MX1, where buffer
solution is added. The pH is automatically controlled from the computer, by means of the pH-meter
AIC 22.1 acting on 22P1.

2.9 SLES deareation unit

The neutralised paste coming from the finishing unit (not included in DBI scope of supply) may
contain a small quantity of air; purpose of deareation is the removing of such air by means of
vacuum, in order to ensure the production of a completely translucent paste.

The high efficiency of the unit allows to modify significantly the specific gravity of the in-feed paste
together with decrease of its apparent viscosity with consequent easier handling and pumping.

The neutralised paste is fed into the deareator 28D1 at controlled rate and thoroughly mixed by a
rotor fitted with a special impeller.

The deareator is maintained at the proper vacuum by means of vacuum pump 28P2.
1E55-40-600 Operation Handbook 17

3. R.M. handling & recommended safety equipment

3.1 R.M. handling

Alkylbenzenes
Alkylbenzenes are combustible materials and should be kept away from sources of ignition, e.g.
naked flames and sparks. The fire risk is in fact only moderate; alkylbenzene will not readily ignite
(flash point typically 120-150°C) but will burn well if it does. Full respiratory protection is needed
when dealing with fires. The vapor is combustible and can explode; all equipment and tanks must
be thoroughly cleaned and cleared as safe before welding is permitted.
Alkylbenzenes are only midly toxic if swallowed, however there is a danger that these low-viscosity
hydrocarbon liquids will tend to break up into a foam if the patient vomits and may therefore be
aspirated into the lungs - a highly hazardous situation. Effects on the skin and mucous membranes
are similar to mineral oils i.e. slightly to moderately irritating, due to their tendency to de-fat the
skin. Inhalation of fumes can have a slight narcotic effect, although inhalation is unlikely at normal
in-use temperatures.
In the case of skin contact, alkylbenzenes should be washed away with water and then with soapy
water. In the case of splashing into the eyes, they should be flushed with copious quantities of
clean water and medical attention sought. No specific guidelines are available for exposure limits
to alkylbenzene aerosol although by analogy with mineral oils a level of 5 mg/m3; 8 hours
time-weighted average is considered appropriate.

Sulfur
The sulfur, usually used in our plants has the aspect of a solid in pieces or in powder, the purity is
included between 99-99.8%.
Its melting temperature is 120°C, its temperature of ignition equal to 226.6°C and its temperature
of autoignition equal to 232°C.
When burning, it produces SO2 which is highly toxic and dangerous.
The sole protection to be taken as regards this product is to stock away from fire sources or from
high temperature, besides, it is advisable to have the ordinary antifire presentation means at one's
disposal.

Caustic soda
It is a product available in the market either as a solid or as a liquid; in the sulphonation plant is
normally used in 40-45% acqueous solution.
The product is highly aggressive and when contacting the skin may cause scalds long to be curied.
When handling , make use of glovers and glasses; in case of accidental contact with skin, wash
with water and a 10% boric acid dermic solution.

SO2 – SO3
In Ballestra plants, the sulfur is brought to the melted state in a day tank and pumped by means of
a dosing pump into a furnace, where its combustion is obtained through controlled air in excess.
The sulfur gas of combustion passes then into a catalyst tower where the transformation of the
SO2 in SO3 occurs.
Sulfur dioxide, sulfur trioxide, sulfuric acid fumes, and oxides of nitrogen normally are not a hazard
in a well operated and maintained acid plant, but all gas fumes can be hazardous to personnel
when proper plant conditions are not maintained. The possibility of equipment failures always
exists.
Sulfur dioxide is a colorless gas having a characteristic odor and a strong irritant action of the eyes,
nose, throat, and upper respiratory tract. A concentration of 3-5 ppm is readily noticed and tasted,
and one of 8-12 ppm causes irrigation of the nose and throat. Coughing and eye irritation are
observed at about 20 ppm.
1E55-40-600 Operation Handbook 18

Higher concentrations are so irritating that voluntary exposure generally cannot be endured. Proper
respiratory devices should be available for entering areas of high concentration and for emergency
purposes.
Sulfur trioxide and sulfuric acid vapors or mists exist as a fog in the air and are irritating to the
mucous membranes of the eyes and respiratory tract. Proper respiratory devices should be
available for emergencies.

LABS
LAB sulphonic acids are eye and skin irritants. When handling sulphonic acids, safety goggles/face
shields, impermeable gloves and protective apron should be worn. A supply of clean, running
water should be available. In case of accident contact, wash off splashes on the skin using copious
supplies of water. With accidental eye contact, wash out the eye with copious supplies of clean
water and get medical attention.

Oleum
It is a dense oily liquid of a greyish color due to impurities contained in the plant.
It is soluble in water when increasing the temperature a lot, it is highly corrosive and, when in free
contact with atmosphere frees SO3 mist.
A great care must be taken when handling and keeping this substance.
If it contacts the skin or the eyes, wash abundantly with 10% boric solution and when the case is
important, undergo a medical inspection.
It is advisable to use protective glasses and gloves and eventually antigas masks with proper filter
for SO3 if this gas happens to leak in the atmosphere.

Primary alcohols and primary alcohol ethoxylated

Primary alcohols are combustible materials and should be kept away from sources of ignition. The
fire risk is considered moderate for detergent type alcohols with flash points in the range 107 -
170°C. The vapour is combustible and may explode; therefore, all equipment and tanks must be
throughly cleaned and cleared as safe before welding allowed.
In the unlikely event of accidental ingestion, drink much water but without inducing vomit.
At normal operating temperatures the vapour pressure is not sufficient to cause inhalation hazard.
Alcohols should be washed from the skin by means of soap and water. In case of splashing into
eyes, wash by means of copious quantities of clean water and medical attention sought. When
handling such materials, goggles and rubber or plastic gloves should be worn.
No specific guidelines are available for exposure limits to alcohols aerosol; altought, by analogy
with mineral oil, considering a level of 5 mg/m3, 8 hour time-weighted average is considered
appropriate.
Alcohols ethoxylated are generally similar to their primary alcohols; therefore, same precautions
and procedures should be followed. In addition, rubber or plastic boots and aprons should be worn
if there is possibility of body contact.

Combustion of fuels.
The start-up burner furnished in this plant utilizes natural gas as fuel. The normal fire and
explosion hazards associated with firing burners with combustible gas will exist if proper operation,
control, and maintenance are not maintained at all times. The possibility of equipment failures
always exists.

Catalyst dust.
During plant operations, the potential for exposure to vanadium catalyst is very low and is not an
hazard. During plant shutdown, when personnel are engaged in handling or screening the
catalyst, a serious hazard results. Exposure to vanadium pentoxide dust produces irritation of the
eyes and respiratory tract. Knowledge of the toxicology of vanadium is incomplete, particularly as
to the chronic and systemic effects. In order to reduce this exposure, it is recommended that the
catalyst is removed pneumatically from the converter and screened externally. In all cases,
personnel should be protected throughout the exposure period with approved respirators and eye
protection. Instructions for screening catalyst are given in spc. SB-PRO-C0001.
1E55-40-600 Operation Handbook 19

Acid burns.
In case of an acid burn, the operator should quickly get under a safety shower and use the full flow
of water; the more water the better. A small amount of water increases the severity of the burn.
Water should be used until all traces of acid have been washed from the burn, normally for a
minimum of 15 minutes. Alkaline solutions are not needed. If used at all, they should be used only
after all acid has been washed from the burn. Once the acid has been washed from the burn, it
may be treated in the same manner as a heat burn.
Safety shower/eyewash stations shall be located during detailed engineering. The showers should
be regularly tested, and maintained when necessary.
Before making any repair on a pipeline or on a flue or piece of equipment that may contain acid,
care should be taken to drain the equipment thoroughly. If a pump line is involved, the pump
should be stopped, the starting switch locked, and the valve suitably closed. Any possible
blockage of the line should be cleared. Maintenance personnel should always have a water hose
nearby, as many burns are avoided or made minor by this simple precaution.

Eye protection.
All operating personnel should wear goggles or eye shields when they are in an area where acid is
being circulated or pumped. This includes, in particular, the area around the drying and absorbing
tower, acid coolers, storage tanks, and loadings platforms.
Goggles or shields must be worn when adjusting valves on acid lines, handling acid, opening a
line, or at any other time when there is even a remote chance of acid leakage or splash. Always
assume that an acid line is full.
A drinking fountain or eye-wash fountain with a liberal upward flow of water is desirable and may
be used to advantage for eye burns. If an operator gets a drop of acid in the eye, the operator
should position the eye directly over the fountain and thoroughly flush it by water. Alkaline
neutralizing agents should never be used for eye burns. It cannot be too strongly emphasized that
the best first aid measure for an acid burn is "A LOT OF WATER QUICKLY!" (It is undesirable to
use a drinking fountain that supplies ice water. It is better to provide water that is not excessively
cold.).

3.2 Recommended safety equipment

Other hazards common to most chemical plants will also exist in this plant and should be included
in accident prevention plans. Some of the common regulations are outlined.
The proper tools for each job should be provided and used. Each operator should wear the proper
safety equipment required for the job performed such as safety glasses, safety goggles, face
shields, acid hoods, hard shell hat, acid proof suit, rubber boots, rubber hat, gloves, welding hood,
respirators, etc.
Specific measures to be taken to eliminate or control each hazard listed in the above analysis
depends upon the owner’s or operator’s attitude for safety and local existing safety requirements in
the acid plant. The owner’s or operator’s personnel will start-up and operate the plant. Ballestra
representatives will adhere to all local safety rules and regulations in force for the owner’s plant
while in the plant.
Safe working procedures are generally developed by a joint venture of the plant workers and the
owner’s safety department. The responsibility for a good safety program rests with plant
management. All workers, operations, and maintenance should perform their respective duties in
accordance with the established safety practices and good housekeeping requirements existing at
the plant site. The recommendations included in the analysis of hazards are the result of past acid
plant experience. One of the most important factors in efficient plant operation is good
maintenance of all operating and control equipment. Annual inspection of all equipment is
recommended. The use of proper materials of construction in making repairs is emphasized in an
acid plant for good accident prevention.
1E55-40-600 Operation Handbook 20

4. Safety prescriptions

4.1 Introduction
The purpose of this part of the document is to provide a support instrument for managing relevant
health and safety concerns relevant to the different kinds of risks at which DBI and customer
personnel can be exposed during pre-commissioning, commissioning and start-up activities and to
provide them information about the prevention and protection measures adopted and the personal
protective equipments to be used during working activities.

4.2 General prescriptions

DBI shall require to the Customer the latest revision of the HSE document about safety prescription
on site, details on PPE required on site, reporting of injuries, incidents and property damage,
location of the nearest medical facility, emergency and evacuation procedure, no smoking
regulations, environmental requirements, cultural and heritage issues.
In case DBI should not receive any communication by Customer regarding any particular risks
related to site operation, DBI will consider that there are no other further risks besides the ones
reported in this document and will communicate it to the Customer.
In this case DBI personnel shall refer to:
1. prescription for behaviour for DBI personnel operating out of office
2. prescriptions for safety and health reported here below

Before leaving for the plant site, DBI personnel will receive from DBI Supervisor a copy of the latest
revision of Customer HSE plan.

DBI personnel will behave as follow once on site :

1. DBI personnel will comply with the requirements of all local laws and standards and Customer
regulation in accordance with HSE document
2. DBI personnel will verify the presence on site of others Suppliers and will request to Customer
regarding risks due to interference; the Customer must assess the overall risk associated with
the simultaneous execution and potential interference of all scheduled jobs and include
additional precautions or measures to guarantee the safety of workers. DBI personnel will report
about any possible interferential risks to DBI Supervisor
3. DBI personnel will identify the Customer Supervisor and he will interface directly and exclusively
with him in order to define how to proceed during pre-commissioning, commissioning and start-
up activities,
4. DBI personnel will report to Customer Supervisor and DBI Supervisor about any equipment
malfunction that may affect the safe operation of equipment,
5. DBI personnel will report to Customer Supervisor and DBI Supervisor about any observations,
particularly about “near miss incidents” or suggestions for risk reduction,
6. DBI personnel will require to Customer that only competent persons are assigned to work tasks.
This includes ensuring the worker has the skills, physique and knowledge to safely execute the
work task.
7. DBI personnel will advise his immediate DBI Supervisor whenever unsure of the instructions for
a task or where concerned about the safety status of any risk
8. DBI personnel will use the PPE provided by DBI / Customer according to the information and
training received.

Anyhow DBI personnel will act with the greatest care and caution to avoid any risk.
1E55-40-600 Operation Handbook 21

4.3 Typical risks

4.3.1 EYE CONSERVATION

In order to reduce the risk for the eye, eye protection shall be mandatory for DBI personnel.
The proper eye protection must be defined in relation with the activity performed and the relevant
risk assessment.
Affected DBI employees shall wear eye (with side shields) and / or face protection where injury to
the eyes or face may be prevented by such personal protective equipment.
The protective lenses /goggles face shields and similar equipments shall be worn in compliance
with Manufacturer requirements and Owner policy.
Each item of protective eye and face equipment shall be properly maintained in sanitary and
reliable condition. The user shall inspect it prior to each use.

4.3.2 NOISE EXPOSURE AND HEARING CONSERVATION

General prescriptions
DBI personnel shall avoid any activity in areas that could represent a risk for hear conservation.
DBI personnel shall use hearing protection when they are exposed to a noise level that exceed
85dBA

Personal Protective Equipments

The following PPE must be used for residual risk:
 Earphones
 Ear plugs

4.3.3 CHEMICAL RISK

General prescriptions
Chemical risk is caused by hazardous substances that are normally used during plant operation
and it can involve DBI personnel during commissioning and start-up operation.
Personnel must be informed about:
 Hazardous chemicals
 Chemical, physical and health hazards
 Exposure limits and ways to control exposure
 Personal protective equipments
 Container labels
Before starting any activity involving hazardous substances collect the Material Safety Data Sheets
to permit a specific risk analysis and the consequent safety prescription.
For hazardous substances which use is not foreseen in DBI Plant, but that are existing on site and
can be source of exposure require MSDS to Customer Supervisor.
Check and verify the position of safety showers, eye showers / wash facilities.
In case of release of an hazardous substance DBI personnel will leave the plant involved area to
avoid exposure.
For safety prescriptions refer also to “Plant Operating Manual – Product Handling” where the effect
of exposure to hazardous substances and the indications about safety measurement to be held in
this case are described.

Personal Protective Equipments

The following PPE must be used accordingly to prescriptions required by the hazardous substance
specific data sheet:
1E55-40-600 Operation Handbook 22

 Protective glasses/ visors

 Gloves resistant to chemical substances
 Protective garments

4.3.4 ELECTRICAL RISK

General prescriptions
Electrical risk can be caused by:
 direct electric contact
 indirect electric contact
 burns due to over temperature
 electric sparks
 electrocuting
 overvoltage
 any other failure condition that can be foreseen reasonably

Before starting any activity that can be a source of electric risk DBI personnel will verify that the
Customer has already performed the grounding system test with positive result.
Before any maintenance operation on any electric powered equipment, electric power must be
carefully shut off and a sign board reporting “electrical works in progress: do not turn the power on”
must be fixed on power control panel.
For activities that must be done over equipment electrically active, it will be necessary to
 use electric tools with protection grade IP55
 use low voltage electric tools
 use electric tool with double insulation
 use PPE for residual risk

Personal Protective Equipments

The following PPE must be used::
 Insulation shoes or boots
 Insulation gloves

4.3.5 MAINTENANCE ACTIVITIES ON EQUIPMENTS

General prescriptions
Risk of injuries to personnel can be caused by maintenance operations over equipments.
DBI personnel shall always refer to the Operation and Maintenance Manual of the equipment
under working.
DBI personnel will not perform directly maintenance activities on equipments that shall be
performed by Customer personnel. DBI personnel will provide supervision services always
referring to the Customer representative.
In case of special reason that will make necessary for DBI personnel to perform directly
maintenance activity, he will operate as follows:
 Communicate to Customer the necessity of technicians for maintenance activities
 Once the Customer has confirmed that he can’t provide any adequate resources DBI personnel
will require to the Customer and to DBI Supervisor the authorization for maintenance activities
 Before undertaking any maintenance activities DBI personnel will have to receive
o Customer authorization
o Authorization and POS from DBI Supervisor
During maintenance activities execution DBI personnel will behave as follows
 Require supervision of Customer representative during maintenance operation
1E55-40-600 Operation Handbook 23

 Shut off electric power to the equipment and take any possible precaution to avoid that the
equipment can be re-started during maintenance operation
 Only after that the equipment has been electrically shut off, remove protection if necessary
 The protection must be removed only for the time necessary to complete the maintenance
 Clearly identify the equipment under maintenance.
 Never let unattended an equipment under maintenance, particularly if the protection has been
removed

Personal Protective Equipments

The following PPE must be used::
 Safety shoes or boots
 Safety gloves
 Protective goggles

4.3.6 LOAD HANDLING

General prescriptions
Load handling can cause risk of injuries due to:
 biomechanical overload, particularly on back-lumbar injury
 osteo - articular injury
 muscular and tendons injury
 nervous and vascular injury
DBI personnel will not perform any load handling but will always refer to Customer representative.
DBI personnel will stay to safety distance from loading / unloading area during load handling.

Personal Protective Equipments

The following PPE must be used for residual risk:

 Safety helmet
 Protective goggles
 Safety boots or shoes

4.3.7 OBJECT OR MATERIALS FALL

General prescriptions
DBI personnel will not stay under areas where job are performed on height and he will keep at
safety distance.
In case it should be necessary to access to such area, it will be always necessary to wear PPE,
particularly the safety helmet.
DBI personnel will take care to never leave on platforms tools that could fall down.

Personal Protective Equipments

The following PPE must be used for residual risks:
 Safety helmet
 Protective glasses
 Safety boots or shoes
 Protective garments
1E55-40-600 Operation Handbook 24

4.3.8 HEAD HITS, FALL, SLIDING AND STUMBLING

General prescriptions
DBI personnel will pay the maximum attention to avoid fall, sliding or stumbling due to the
presence of falls, holes, materials left on the working areas or head hits against structures or
obstacles
DBI personnel will refer to Customer representative to signal the presence of materials that could
cause risk of falling.
In case of access to equipment located at more than 2 mt above ground, DBI personnel will verify
the use of primary fall protection systems, such as scaffolds, aerial lifts, personnel hoists, etc...
Fall protection equipment must be inspected before each use.
If DBI personnel should evaluate that fall protection system are not satisfactory in terms of safety,
he must not access to the relevant equipment.

Use of ladders should be avoided; the use of ladders properly designed, constructed and approved
by Customer may be acceptable in limited applications. In such cases DBI personnel shall verify as
minimum:

 The ladder must be approved by Customer HSE office

 The use of metal ladders will be limited and wood or fiber-glass ladders are preferred. Metal
ladders shall not be used if the might become energized
 The ladder must be equipped with non-slip feet
 Ladders for egress and/or to conduct low level work of short duration is acceptable, but ladders
may not be used in lieu of scaffolds as a primary means of conducting work of longer duration,
or stairways
 Ladder shall have a minimum width of 0.3 mt
 The spacing of ladder rungs is uniform and between 0,25 and 0,3 mt
 Ladders must be inspected prior to each use.
 Ladder in use shall be free of oil, grease or other slipping hazard
 Ladder are always tied at top to a secure object
 An employee on a ladder should not carry any object or load that could cause the worker to lose
balance and fall; all tools or materials should be hoisted or lowered by a hand line
 Ladder extend at least 1 mt above the upper landing surface
 The area around the top and the bottom of the ladder must be kept clean
 A ladder in use has an angle greater of 75° from vertical
 When ascending or descending the ladder the employee faces the ladder and has three-point
contact all times

Personal Protective Equipments

The following PPE must be used for residual risk:
 Safety shoes of boots
 Safety helmet

4.3.9 BURNS

General prescriptions
Burn injuries can be caused by contact with hazardous substances (refer to par. “Chemical Risk”)
or with contact with hot surfaces.
DBI personnel will avoid contact with hot surface referring for identification to DBI Plant
engineering documents for all included in DBI scope of supply, and to Customer representative for
all not included in DBI scope of supply.

Personal Protective Equipments

The following PPE must be used for residual risk:
1E55-40-600 Operation Handbook 25

 Safety gloves

4.3.10 VESSELS AND CONFINED SPACES

General prescriptions
DBI personnel should avoid to enter inside vessels or confined spaces.
In case of special reason that will make necessary for DBI personnel to enter inside vessels or
confined spaces he will operate as follows:
 Communicate to Customer the necessity of technicians for activities that requires to enter
inside vessels or confined spaces
 Once the Customer has confirmed that he can’t provide any adequate resources DBI personnel
will require to the Customer and to DBI Supervisor the authorization for the activity
 Before undertaking any maintenance activities DBI personnel will have to receive
o Customer authorization
o Authorization and POS from DBI Supervisor
Before entering in the confined space DBI personnel shall ensure that:
 A hazard assessment has been performed and documented on a Safe Work Permit prior to
entry.
 Atmospheric testing (oxygen content, flammable gases and vapors and potential toxic air
contaminants) will be conducted on all confined space prior to entry and written documentation
shall be maintained.
 All energized piping systems shall be locked or blocked and tagged to isolate contaminants
and energy and all electrical sources shall be isolated.
 Only low voltage or Ground Fault Circuit Interrupter (GFCI) controlled electrical power shall be
used,
 Some personnel shall be appointed as “safety watcher” (confined space attendants); they will
be easily identified, competent and aware of the duties associated with each emergency
situation that may occur within the confined space
 A safety watcher shall be present at all times.
 An emergency rescue team shall be available for all confined space entries and that all
employees know how to summon assistance.
 Employees who are to enter a confined space are properly instructed, and trained in the use of
protective equipment, if applicable.
 To have stand by or available on site the appropriate extraction equipment and personnel
trained in rescuing people from confined spaces
 Oxygen - % and % LEL are monitored, and that warning systems are in place if safety margins
are exceeded; in case safety margins can not be maintained independent air/breathing
equipment is mandatory.

Personal Protective Equipments

The following PPE must be used for residual risk:
 Safety gloves
 Safety glasses / visors
 Safety garments
 Safety boots / shoes
 Air breathing equipment (if required)

4.3.11 PERSONAL PROTECTIVE EQUIPMENTS

GENERAL REQUIREMENTS
All personal protective equipments must be CE marked or approved according to local
Regulations.
1E55-40-600 Operation Handbook 26

All personal protective equipment utilized at work shall be properly maintained in sanitary and
reliable condition and shall be inspected by the user prior to each use. This requirement is
mandatory.

In case PPE shall be provided to DBI personnel by Customer, DBI personnel shall be trained in the
correct application and use of personal protective equipment. This shall be certified, in writing, by
individual identity.
DBI personnel will inform DBI supervisor about PPE and relevant training (if any) received by the
Customer and will follow DBI prescriptions / instructions about their use.

Every employee will at all times wear clothing that protects the body and extremities. The typical
personnel hazards listed below can be prevented as follows:
 Thermal burns resulting from contact with hot pipes, can be prevented by using long sleeve
shirts and cloth gloves.
 Chemical burns and/or skin absorption of allergens and toxins can be prevented or minimized
by use of appropriate chemical protective clothing.
 Loose clothing will not be worn where it can contact or catch on energized conductors, moving
parts, equipment, or other hazards of this type.
 Preference should be given to natural fibers in the clothing worn by personnel.
 Short pants are prohibited as outerwear.
 Finger rings or necklaces are prohibited when there is a danger of catching them on moving
parts or contacting an energized conductor.

Personnel working on plant shall wear:

 Safety – steel toed footwear (shoes or boots)
 Safety glasses with side shields
 Safety hard hat or helmet
 Others PPE if required accordingly to risks at which they are exposed during plant activities

All PPEs that have been subject to events that could jeopardize their effectiveness (for example an
hit or a fall) must be substituted even if they don’t show any visible deficiency .
 1E55-40-600 OPERATION HANDBOOK 27

PERSONAL PROTECTIVE EQUIPMENT MATRIX

Activity Hazard Threat FP HH SG G FS HP SB Comments

Hits, falls,
sliding,
1 Plant
Site access struck M M R M
environment
against or
on
Lifting
Sharp edges,
2 Handling injuries,
splinters, rough M M M M
material lacerations,
surfaces
punctures
Working at Verify the existence and
3 Working at Fall on or height over 2 mt quality/effectivness of primary
M M M R R M
height onto or above rotating PPE (scaffolds, personal hoists,
systems ecc…)
4 Stuck by objects
Pressure test Hits, falls M M M
/ flying pieces
Refer to equipments
Mechanical
Sharp edges, maintenance and operating
pre- Injuries,
5 splinters, rough manuals. Shut-off electric
commissioning lacerations, R M M M R M
surfaces, power before any maintenance
general burns
electrical contact operation on electrically
activities
powered equipment
Contact with
Check safety measures to be
toxic agents,
Dermatitis, undertaken in case of exposure
6 Line flushing contact with hot
blisters, R M M M R R M to chemical agents, do not
activities surfaces, stuck
burns, hits touch lines in case of steam
by objects / flying
flushing
pieces
Refer to equipments
Alignement Sharp edges, maintenance and operating
Injuries,
7 and splinters, rough manuals. Shut-off electric
lacerations, R M M M R M
lubrification of surfaces, power before any maintenance
burns
machinery electrical contact operation on electrically
powered equipment
Check that the ground test has
been performed successfully,
Electrical Burns, refer to relevant maintenance
8 Electric contact M M M M and operating manual, use
procedures fulmination
electric tools with protection
IP55, use electrical tools with
double insulation
Contact with Check safety measures to be
Dermatitis,toxic or corrosive undertaken in case of exposure
9 Start-up blisters, agents, contact R M M M R R M to chemical agents, do not
burns, with hot touch lines during plant
surfaces operation
KEY: HH: hard hat / helmet. SG: safety glass/goggles (all glass shall have side shields). G: Gloves (hand protection shall be carried and
available for use). FS: face shield. HP: Hearing protection. SB: safety boots / shoes (they shall have puncture resistant soles). FP: Fall
protection. M: mandatory. R: may or nt may mandatory according to activity.
 1E55-40-600 OPERATION HANDBOOK 28

5. Pre-commissioning

5.1 Check list for plant completion

(Mechanical Supervisor)

A. Carry out a general inspection of the PLANT, in order to check conformity with
flow diagrams, VENDOR prints, specifications, civil drawings, codes and
standards.

B. Assist the CUSTOMER (if required) during collection of all permits and
certifications released from local insurance or governmental agencies, concerning
occupancy and operation of the PLANT.

C. Obtain the manufacturer's (VENDOR) assistance to ensure satisfactory

installation of equipment. Provide manufacturer's (VENDOR) assistance, if
required, for pre-commissioning or run-in machinery.

NOTE: The Client will provide (under request) to inform the Vendor/Manufacturer
about the plant working progress by means of a planner.

5.2 Pressure test

Purpose

The allowed pressure test types are as follows:

- hydraulic check
- pneumatic check at full pressure

Usually the pressure test of the laying piping has to be performed with the hydraulic
check.

The pneumatic check at full pressure replaces hydraulic check when the hydraulic check
fluid into the piping could cause the following troubles:

- damage the inside lining

- cause damages for freezing owing to low ambient temperatures.
- be prejudicial to be process owing to pollution caused by test residual fluid
- be prejudicial to material (corrosion) owing to presence of residual test fluid
- cause the permanent deformation of the lines because of the fluid weight,
especially the lines of big diameter and thin thickness.
- cause excessive overload of the supporting structure.

Before pneumatic check, non destructive checks of all welded joints have to be carried
out. Since compressible fluids are used, the pneumatic check involves some risks, in
case of failures or sudden leaks. Therefore, the limit values indicated in the following
table 1 have not to be exceeded.
 1E55-40-600 OPERATION HANDBOOK 29

WARNING!
Danger of explosion due to pressurization of lines and equipments.
Area of piping under test must be limited and a sign board indicating
“pressure test in progress” must be provided.
During the test execution all non-concerned personnel has to be moved
away from the area of piping under test and kept at safety distance.
Pressure test must be performed according to the specified procedure.
Personnel in charge of pressure test that access to the test area, must
wear personal protective equipment for residual risk (refer to Safety
prescription for pre-commissioning, commissioning and start-up activities)

The equipment can be divided into two main groups:

Group A All process lines for air/SO2/SO3/exhaust gas starting from the main blower
to the caustic scrubber as well as the cooling air & hot air lines belong to
this group. The “pneumatic” test is required for this group of lines.

Group B This group includes all the process lines and utilities lines except the ones
belonging to the group A. The “hydraulic” test is required for this group of
lines.

Test execution

The tests have to be performed on the piping not painted in the welding areas and
without thermal insulation or any outside coating.
All the joint surfaces have to be dry, without dirt and/or grease. This is necessary to allow
the test and check of possible leakage and bleeding of the test fluid.

Before performing any test, the following components will have to be excluded from lines,
as they could be damaged:

- Diaphragms, calibrated orifices, Venturi pipes, rotameters, meters and any in-line
instrument;
- Filters and filtering elements;
- Instruments and related connection lines to the process;
- Piping operating with free discharge on working (e.g. vents & discharges) have to be
disconnected;
- Break disks, pressure reducing valve, safety valves;
- Expansion joints, below or telescopic type (if not blocked);
- Control valves.

The above mentioned line components, the equipment and machinery will be isolated
from the piping by interposing blind disks or will be removed.
In the first case, the tang of the blind disks has to be painted to facilitate their
identification when removing them at the end of the test; in the second case, in order to
replace the removed components, some temporary pieces or blind flanges or threaded
plugs have to be assembled which have to be taken away after emptying.
 1E55-40-600 OPERATION HANDBOOK 30

The blind flanges have to be removed to effect emptying.

TABLE 1 - DETERMINATION OF THE TEST PRESSURES

TEST TYPES LINES GROUP CALCULATION OF TEST

PRESSURES
ANSI
Pneumatic A Ptp = Pd x 1
Pti = Pd x 1.5 *
Hydraulic B
Pti = Pd x 1.5 x  /p **

Where:

Pd = Design pressure indicated on the lines list

Ptp = Pneumatic test pressure
Pti = Hydraulic test pressure
= Allowable stress (of the line material with the lowest mechanical
characteristics) at test temperature
p = Allowable stress (of the line material with the lowest mechanical
characteristics) at design temperature.

** = Formula to be used when the design temperature is lower than the

presumable temperature of the hydraulic test.
* = Formula to be used when the design temperature is higher than the
presumable temperature of the hydraulic test, however when the design
temperature is higher than 30 degree C

Hydraulic check

Test fluids

Generally, water at ambient temperature has to be used. The quality of water has to be
selected depending on the characteristics of the piping material, as follows:

Demineralized or condensate water (however with chlorides content lower than 30 ppm)
is employed for lines in stainless steel, aluminium and its alloys. Water containing from
30 up to 100 ppm of chlorides can be used in case of need, provided that either the
operating temperature of the line is lower than 50° C or the lines are flushed with
chlorides-free water after test.

Well water is employed for lines in carbon steel, low alloy steel, copper and its alloys,
titanium and its alloys; it is always advisable to have the chemical analysis of the well
water, in order to check its suitability for the use.
 1E55-40-600 OPERATION HANDBOOK 31

Lines preparation

Generally the test is performed on one line at a time. However, two or more lines can be
combined, compatibly with their design conditions and the resistance of the support
structures, to build-up a system to be tested on the whole.
The lines with reduced jacket must be tested before and after jacketing.
The underground lines within battery limits must be tested before being layed
underground.

On the lines to be tested, which have not been designed to support the weight of the test
liquid, some temporary supports (not welded) must be installed in order to avoid any
possible overload damage.

The big diameter and thin thickness lines, having supports located at great distance one
another, have not to undergo the hydraulic tests in order to avoid lines damage.

The lines list has to point out the lines which have not to be tested for the above
mentioned reasons.

All shut-off valves which remain in line shall have the shutter fully open.

The lines containing check valves should have the source of side pressure upstream, i.e.
the filling has to be made according to the operating fluid direction. If this is not possible,
it is necessary to block on inlet or take off the shutter. If also this is not possible or
however not advisable, then the valves have to be removed or replaced with temporary
pieces.

Before testing, block all the elastic supports and expansion joints, not excluded from the
lines.

Remove the caps or end flanges and open the relief valves on all vents and drains.

If not provided on the design drawings, install some vents and drains required for the test
execution on the highest and lowest points of the lines to be tested.
If they cannot be installed on the pipe for problems of welding or material damage, they
have to be installed on the blind flanges located upstream and downstream the lines.

On the lowest point of the piping system to be tested, install two manometers in parallel.
In case it should be not possible to install them on the lowest point, the pressure head
will have to be considered during pressing operation.
These manometers shall have full scale equal to 1,5 the test pressure, and have to be
calibrated before starting the test.

On the test fluid feeding pipes, install a filter in order to avoid any inlet of foreign matters
into the lines, during the filling and pressing operations.

The hydraulic test has not to be performed with outside wet piping and above all, on
lengths of piping in the open air the test has not to be performed when raining.
Such test has not to be carried out also when ambient temperature is lower that 4°C.
In any case it is recommended that the temperature of steel components takes the
nearest possible value as the test fluid, before going on with the pressing operation.
 1E55-40-600 OPERATION HANDBOOK 32

If high ambient temperatures and/or a long exposure time of the test lines can vary the
fluid temperature and cause pressure variations, suitable precautions have to be taken to
avoid that it may change the results of the test, or cause dangerous conditions by
stressing the materials beyond the yield point.

Filling

The filling has to be provided from the lowest points of the lines and it will be necessary
to vent all residual air contained in the lines. When filling is complete, all vents have to be
closed.

Pressing

Pressing of the lines has to be effected gradually, stopping at intermediate values for the
time required to uniformly stress the whole line and the system.
The test pressure has been considered reached, when the value indicated on the lines
list can be read on the manometers.

Test

The test pressure has to be kept for at least one hour before performing the inspections.
Proceed to:

- Check of the test pressure value (on the manometer), which has to remain constant
for all duration of the test.
- Visual check of the welding in order to identify leaks, if any.

In case leakage or bleeding are detected, the welding will have to be remade.
After repairing, the hydraulic test has to be repeated with the same procedure.
- Visual check of the flanged and/or threaded connections in order to ascertain leaks, if
any.
In case of leaks from such connections the bolts and/or threaded connections will
have to be tightened; if not sufficient, it will be necessary to verify the perpendicularly
of the flanges faces as to the pipe axis, and to check the seal surfaces of the flanges.
If necessary, they will be replaced and however the gaskets will be replaced; then the
test will be repeated.

Pneumatic check

Test Gas

Generally, air at ambient temperature is used.

When the presence of oil or moisture is not allowed in the lines, it is necessary to use dry
air (instrument air) or nitrogen.
 1E55-40-600 OPERATION HANDBOOK 33

Test Pressure

The test pressure is indicated in the Lines List; failing this indication, proceed as per
above indicated TABLE 1.

Lines/equipment preparation

The lines/equipment preparation is generally the same as per the above indicated
hydraulic test procedure, except for the location of the manometer, which is for the
pneumatic test.

Pressing

Pressing of the lines has to be effected gradually, stopping at intermediate values for the
time required to uniformly stress the whole line and the system.
The test pressure is to be considered as reached when the value indicated on the lines
list can be read on the manometers.
Pressing has to be performed taking all the required precautions, in order to avoid any
sudden gas leak (due to joints failure, or any other reason) that could lead to personnel
injuries or property damage. Particularly, the pressing operation must be accomplished
by gradually increasing the pressure, step by step (each step increase not to exceed 0.25
bar).

Test

The test pressure has to be kept for at least one hour before performing the inspections;
therefore the following checks have to be effected:

- Check of the test pressure value (on the manometer), which has to remain constant
for all duration of the test.
- Visual check of the welding, in order to identify leaks (any gas leak will be noticed
once spreading a soapy solution on the flanges or welding connections).
- In case leakage or bleeding are detected, the welding will have to be remade.
- After repairing, the hydraulic test has to be repeated with the same procedure.
- Visual check of the flanged and/or threaded connections in order to ascertain leaks, if
any.
In case of leaks from such connections the bolts and/or threaded connections will
have to be tightened; if this is not sufficient, it will be necessary to verify the
perpendicularly of the flanges faces as to the pipe axis, and to check the seal
surfaces of the flanges.
- If necessary, they will be replaced and however the gaskets will be replaced; then the
test will be repeated.

Pre-commissioning activities are the non-operating adjustments and cold alignments

checking.
Since the situation differs from plant to plant, depending on the progress of the erection
and the layout of the plant, only general guidelines are given. On the basis of these, a
detailed working program will have to be drawn up.
 1E55-40-600 OPERATION HANDBOOK 34

5.3 Mechanical procedures

General activities

- Carry out a general inspection of the plant, to check conformity with flow diagrams,
construction drawings, piping arrangement, vendor prints, civil drawings and
specifications, codes and standards and Ballestra specifications.
- Arrange for any special prestart-up inspection as required by Government and/or
insurance agencies.
- The customer should organize, with mechanical supervisor help, the warehouse of
spare parts and maintain the necessary records.
- Verify and approve works progress and plant check; control any exceptions and note
on a separate work order list (punch list).
- Remove all rust preventives and oils used to protect the equipment during the
construction period whenever these protective materials will be detrimental to
operation.
- Remove all temporary supports, bracings or other foreign objects that were installed
in vessels, rotating equipment, electrostatic precipitator or other equipment to prevent
damage during shipping, storage and erection.
- Customer should check on Mechanical Handbook and provide a list of available
lubricants to be used in the plant; the list should be approved by Mechanical
Supervisor and the initial charge of them should be added
- Install mechanical seals, permanent packing and accessories where required.
- Check rotating machinery for correct direction of rotation and for freedom of moving
parts before connecting driver.
- Make cold alignment to the manual's instruction tolerance.
- Make non operating field leak test or field pressure test on piping and field fabricated
equipment.
- Prepare all system for safe tie-ins.
- Conduct all operational tightness testing.
- Test and adjust all safety devices, seal wherever necessary for internal rules or
desirable and install them (including pressure-relief valves).
- Flush and clean lines and equipment (see chapters Flushing activities and Specific
Procedures).
- Remove all steam traps and flush heating lines and coils with steam for at least 1 day.
- Provide continuous clean up of the construction area; remove excess materials.

WARNING!
Refer to equipment maintenance and operating manual for safe operation
and to avoid damaging to the equipments.
Wear personal protective equipment, i.e. safety helmet, safety gloves,
safety boots or shoes, for residual risk.
 1E55-40-600 OPERATION HANDBOOK 35

Flushing activities

In order to remove all foreign matters, the process side of the installation should be
flushed with water. Use of other liquids or gases (air or nitrogen) is also necessary.
Before starting the cleaning procedure, make sure that all raw material inlet lines have
been blanked off at battery limits.

Requisites for flushing:

- sufficient water of the correct quality (flushing water should be cleaned with no
suspended solids).
- hoses with appropriate couplings
- sufficient compressed/instruments air, oil free.
- conical filters and blanks.
- sufficient spool pieces.

Blanks as well as filters must be provided with lips or other markers projecting from the
flanged joint so that they may easily be found back.

Care should be taken that the temperature of the flushing liquid does not exceed the
maximum operating temperature of the equipment concerned.

Flushing by water

- Uncouple lines at control valves, flow meters and pumps.

- Remove all process filters, orifice plates, flow totalizers and non-return valves.
Replace them with spool pieces.

Lines:
- Velocity of the flushing water should be in the range 2-4 m/sec (6.5-13 ft/sec).
- Where possible, flush from top to bottom.
- Start with main lines and pump suction lines.
- If possible, flush in the direction away from process equipment.
- Should this be impossible, uncouple lines at these items.
- Flush separately "dead" sections, e.g. by-passes around control valves,
rotameters, pockets in lines.
- Check if uncoupled lines can be easily, without tension reconnected to other
lines, pumps, vessels, etc.

Pumps:
- Clean thoroughly and prepare for operation.

Process equipment:
- Fill completely and drain as rapidly as possible; during drainage, ensure proper
venting, so that no underpressure can develop.
 1E55-40-600 OPERATION HANDBOOK 36

Flushing with other liquids

If the lines and/or process equipment items are seriously fouled, it may be necessary to
flush with solvents. If oils and greases must be removed, flushing should be done with
hot water at 60-80° C.

After the flushing described above, circuits are established and water is circulated
through them by the process pump. Filters should be checked regularly and, if
necessary, fresh water must be taken. After through flushing, the installation is drained
and internally cleaned where necessary (e.g. tanks and other vessels).

This after flushing must be carried out as soon as possible after flushing of the separate
parts.

WARNING!
Chemical risk can be caused by hazardous substances used for flushing.
Check substance MSDS for related risk, exposure limits and safety
measures to be undertaken in case of exposure.
Check the location of emergency shower.
Wear personal protective equipment during operation for residual risk
(refer to MSDS and to Safety prescription for pre-commissioning,
commissioning and start-up activities)

Purging with gases

Air:
- Remove impurities by means of an air stream from lines which cannot be flushed with
water for process, mechanical or dimensional reasons.
- The velocity of the oil free and dry stream should be in the range 15-20 m/sec. (50-65
ft/sec.); if this velocity cannot be reached, other procedures will have to be followed.
- It is possible, for instance, to pressurize the line with air or nitrogen to the maximum
allowable pressure (see data and lines sheets) and then to release the pressure
suddenly.

WARNING!
Danger of explosion due to pressurization.
During the test execution all non-concerned personnel has to be moved
away from the area of piping under test and kept at safety distance.
Personnel in charge of operation must wear personal protective equipment
for residual risk (refer to Safety prescription for pre-commissioning,
commissioning and start-up activities)
 1E55-40-600 OPERATION HANDBOOK 37

Steam:
- In general, only steam and condensate lines are to be subjected to a steam purging.

WARNING!
Danger of burns and injuries due to thermal contact.
During the operation all non-concerned personnel has to be moved away
from the area of piping under test and kept at safety distance.
Do not touch lines during steaming.
Personnel in charge of operation must wear personal protective equipment
for residual risk (refer to Safety prescription for pre-commissioning,
commissioning and start-up activities)

Actions to be taken after flushing

- Remove all blanks used for flushing purposes, except the blanks in raw materials inlet
lines.
- Install process orifice plates, process filters and non return valves.
- Connect all control valves, flow meters, pumps, vessels etc.
- Check if uncoupled lines can easily, without tension, be reconnected.
- Where possible, the conical filters used during the flushing procedure should be left in
the process lines.
- Be sure they are clean and have been installed in the proper position.

Leak test

The leak test of all process equipment and lines which are jacketed must be done after
the entire steam system have been heated to the operating values and then cooled
down.

All the flanges in the process and heating system have to be tightened again.

In order to carry-out the leak test, the plant must be divided into parts which can be
tested separately.
Then all equipment, including the connected lines, must be leak tested with nitrogen or
air.

In case the system is not protected by safety valves, the pressure of the nitrogen (or air)
must be limited to such a value that the design pressure of the equipment cannot be
exceeded (see data and lines sheets).

Care should be taken that the mechanical seals of agitators and pumps are not
damaged.

All test will be conducted in accordance with applicable codes and specifications.
When the test will be completed:

- Provide test records for CLIENT

 1E55-40-600 OPERATION HANDBOOK 38

- Witness tests when notified by CONTRACTOR

- Conduct all operational tightness testing
- Repair any leaks resulting therefrom

WARNING!
Danger of explosion due to pressurization.
During the test execution all non-concerned personnel has to be moved
away from the area of piping under test and kept at safety distance.
Personnel in charge of operation must wear personal protective equipment
for residual risk (refer to Safety prescription for pre-commissioning,
commissioning and start-up activities)

Alignment and lubrication of machinery

Lubricants

- Customer should check on Mechanical Handbook and provide a list of available

lubricants to be used in the plant; the list should be approved by Mechanical
Supervisor and the initial charge of them should be added
- Flush systems if required by Vendor and dispose of flushing fluids in accordance with
CLIENT's instructions.
- Provide records of initial charge of all lubricants.
- Maintain lubrication after initial charge.

Packing and Seals

- Install mechanical seals, permanent packing and accessories when required.

- Witness above installation
- Make adjustment and replacement to mechanical seals, packing and accessories for
alignment

Rotation and Alignment

- Check rotating machinery for correct direction of rotation and freedom of moving parts
before connecting driver.
- Provide records of the rotating machinery checked.
- Perform cold alignment to manufacturer's tolerance
- Witness tests.

WARNING!
Refer to equipment maintenance and operating manual for safe operation
and to avoid damaging to the equipments.
Wear personal protective equipment, i.e. safety helmet, safety gloves,
safety boots or shoes, for residual risk.
 1E55-40-600 OPERATION HANDBOOK 39

Filling of inventories

The inventory of the sulphonation plant consists of:

Ethylen glycol solution at 20% as concentration (item 11V3)).
A) Moisture absorber material (silica gel and activated allumina) for 11C1.
B) SO2-SO3 converter material (vanadium pentoxide) for 12C1.
C) Refractory material for sulphur furnace (item 12H1).
E) Packing material (pall plastic rings) for scrubber 14C1.

Provide all the inert packing materials and beds materials, such as a sand, gravel, balls
and saddles; provide the operating materials for equipment such as chemicals, resins,
dessicants and catalyst.

Inspect the vessels inside, before assembling the internals and loading; the loading
activities should be witnessed, in order to ensure the correct installation and conformity to
the recommended procedures.

5.4 Electrical procedures

Electrical Power and Lighting System

Notify CLIENT of test schedule.

- Witness tests when notified and record test data if desired.
- Perform insulation test of wiring using a megohmmeter where applicable.
- Perform insulation tests of motor windings and of transformer windings.
- Perform grounding system tests to determine continuity of connections and value of
istance to ground.
- Obtain local inspectors approval when required. Obtain approval from local officials
when required.
- Check phase sequence and polarity.
- Check installation of emergency power systems.
- Check all motors for rotation.
- Check all lights and check levels for adequacy.
- Check all control circuits for proper operation.
- Provide CLIENT with record of work completed.
- Take over responsibility for maintenance of energized electrical facilities upon
acceptance by CLIENT as mechanically complete.
- Issue permits to CONTRACTOR for carrying out checks on electrical facilities which
are energized.

Instrument Systems

Make non-operating checks to ensure instrument operability, i.e. remove all shipping
stops, check pointer travels and certify instrument capability to measure, operate and
stroke in the direction and manner required by the process.
- Field calibrate instruments with standard test equipment and make all required
adjustment and control point settings.
- Fully pressurize and energize the transmitting and control signal system, opening
process connections at primary sensors and final regulators.
 1E55-40-600 OPERATION HANDBOOK 40

- Make control mode settings and other adjustment to systems for automatic operation
of equípment.
- Install and connect all system components and verify their conformity with
specifications and design criteria for function and range using dummy transmitted
signals as needed.
- Clean all transmission and control tubing by blowing with cooled and filtered clean air
prior to connecting to instrument components.
- Clean all air supply headers by blowing with clean air prior to connecting to instrument
components.
- Perform leak tests of pneumatic control circuits.
- Check process lead piping for tightness.
- Check all electrical signals and alarm wiring for continuity, correct sources of power
and polarity.
- Check thermocouples for proper joining of wires, position of elements in wells, proper
polarity and continuity of receiving instruments.
- Insulate, or remove if necessary, inline components such as control valves, positive
displacement meters, turbine meters, etc., for pressure testing and re-install them.
- Check bores of orifice plates.
- Install such plates after completion of flushing operations.
- Insulate or remove in-line components for flushing operations and re-install them on
the completion of such operations.
- Test all relief valves if required and tag them with stainless steel tags.

WARNING!
Danger of burns and/or folgoration due to electrical contact.
For any operation on electrically powered equipment or instrument:
- Check that the ground test has been performed successfully
- refer to relevant maintenance and operating manual
- use electric tools with protection IP55
- use electrical tools with double insulation
- use PPE for residual risk.
Before any maintenance operation on electrically powered equipment, shut-off
electric power and fix a sign board reporting “electrical works in progress: do not
turn the power on” on power control panel.
 1E55-40-600 OPERATION HANDBOOK 41

5.5 Computer procedures

General activities
In this section the TEST and/or PRE-COMMISSIONING activities related to the control
system of the plant are described.
Check connections between PC and PLC:

a. Check installation of the connecting cables between the following equipment:

- Feeding: UPS - PLC panel board
- PCs Control Room: Personal Computer/Printer located in control room from
PLC panel with cable installed in the CABLE TRAYS
- Bus cables: some terminals of the bus cables DH+ and Ethernet (if existing)

b. Check following functions:

- Communication between PLC and the remote racks i/o (the communication cards
placed in each rack should be set correctly before starting this operation)
- Communication between the PLC and the PC located in the Control Room on
line Data Highway Plus (DH+)

The scope of the above activities is to check the correct connection of the units which are
part of the control system.

Plant I/O test

The check of the correct connections of the electric, electronic equipment installed in the
plant has to be carried out in 2 main activities, that are:

- I/O test analog dígital from field to terminal box (barriers if existing) of the
PLC cabinets, by means of a computer that Ballestra will use for the control
of the PLC software located in the Control Room).
- I/O analog digital tests viewed and commanded from the control computer.

In general the I/O test has to be carried out following the selection of the sections
componing the plant indicated here below:

- Section 11
- Section 12
- Section 14
- Section 16
- Section 17-22
- Section 25
- Section 28
- Section 07

General functionalities test

After checking the correct correspondence between the plant I/O and the same
commanded from the Computer Control System, it is possible to proceed with the
General Functionalities Test of the system, such as:

- Interblocks
- Loop PID
 1E55-40-600 OPERATION HANDBOOK 42

- Manual Micro Sequences

- Emergency interlocks
- Alarms
- Historical trends
- Actual trends

5.6 Special equipment procedures

Inspect for completeness and correctness of installation and make all required non-
operating checks.

AIR DRYING UNIT (item 11C1 )

Make reference to the enclosed Ballestra Standard Procedures.
(Spec.: SB-PRO-C0002 – AIR DRYING UNIT).

SULPHUR FURNACE CURING (item 12H1 )

Make reference to the enclosed Ballestra Standard Procedures.
(Spec.: SB-PRO-H0001 - SULPHUR FURNACE).

SO2 / SO3 CONVERTER COLUMN (item 12C1)

Make reference to the enclosed Ballestra Standard Procedures.
(Spec.: SB-PRO-C0001 - SO2 / SO3 CONVERSION COLUMN).

SO3 COOLERS (item 12E5/6)

Make reference to the enclosed Ballestra Standard Procedures.
(Spec.: SB-PRO-E0001 – CLEANING PROCEDURE FOR SO3 COOLERS).

SO3 FILTER (item 16F3)

Make reference to the enclosed Ballestra Standard Procedures.
(Spec: SB-PRO-F0003 - SO3 BRINK FILTER).

FILM REACTOR (item 16R1)

Make reference to the enclosed Ballestra Standard Procedures.
(Spec.: SB-PRO-R0001 - FILM REACTOR PRE-COMM./COMM.&MAINTENANCE).

ESP (item 14F1 )

Make reference to the enclosed Ballestra Standard Procedures.
(Spec.: SB-PRO-F0001 ESP ELECTROSTATIC PRECIPITATOR - ITEM 14.F.1 -
MECHANICAL HANDBOOK.)

MOLTEN SULPHUR TANK (item 25V1)

Make reference to the enclosed Ballestra Standard Procedures.
(Spec.: SB-PRO-V001 - SULPHUR MELTING TANK - ITEM 25.V.1 - OPERATION &
MAINTENANCE HANDBOOK).

NEUTREX MIXER 33MX1 MECHANICAL SEAL PRESSURE VESSEL

Make reference to the enclosed Ballestra Standard Procedures.
(Spec.: SB-PRO-MX001 - START-UP PROCEDURE FOR OPPOSED DOUBLE
MECHANICAL SEAL STIRRERS (BALANCED TYPE)
 1E55-40-600 OPERATION HANDBOOK 43

SO2 SCRUBBER COLUMN (item 14C1 )

The first assembly action is the vertical positioning of the vessel on the concrete base and
the fixing through the concrete foundation bolts.
After 48 hours from the bolt phase, the internals assembly can begin.

1) Open the manhole ; assemble the lower grid and fix the plastic net, by means of nylon
binding.
2) Close the manhole .
3) Load the pall rings from the sight manhole , up to the altitude indicated in the data
sheet..
4) Cover with the plastic net and insert the grid supplied in sectors to be connected with
nylon, in order to avoid any movement of the packing material during operation.
5) Install the liquid distributor over the packing material through the nozzle S3 and S4a;
verify the correct vertical position of nozzles (position C).
6) Assemble the upper grid and fix the plastic net, by means of nylon binding.
7) Open the top flanged cover of the column S2; load the pall rings from the sight
manhole S2, up to the altitude indicated in the data sheet (position A). At the end
reassemble the top cover S2.
8) Install the teflon pipe in the nozzle S6 (oleum inlet), so that the tube is turned
downwards.

WARNING!
Danger of fall from elevation.
Refer to Safety prescription for pre-commissioning, commissioning and start-up
activities.
Use of personal protective equipment is mandatory.

GLYCOL TANK (item 11V2)

The only operations to be done is the dilution of the concentrated ethylen glycol (supplied
in steel drums), directly in the vessel through the nozzle S11.
Required concentration and glycol - water quantity are indicated in the data sheet.

METERING PROPORTIONING PUMPS

Even if each metering pump is supplied from the manufacturer with the relating "Test
Certificate", a calibration on site is required after the positioning, to establish and/or
confirm the real flowrate .

Normally, in the Ballestra plants, all the metering pump delivery lines are provided with a
drain pipe with a valve suitable for the calibration control.

Equipment required:

- Stop watch.
- Weighing scale, 0 - 5 Kg.
- Plastic containers
- Weighing scale, 0 - 50 Kg.
- N° 2 Metallic containers (for sulphur pumps).
 1E55-40-600 OPERATION HANDBOOK 44

Procedure

1 Where it is possible, connect the drain pipe with the feeding tank and use the suitable
process liquid for which the pump is installed.

 If it is not possible to recycle in the feed tank, provide to make use of a drum to
collect the liquid.
 If the process liquid is not available, make use of water and convert the results
to the process fluid (knowledge of process fluid density is necessary).

2 Start pump motor.

3 Regulate the piston length at 20% (by the proper mechanism), wait 2-3 minutes to
stabilize the flow and determine the out-flow, by weighting a sample for a known time
(usually 1 minute).
Repeat the operation with the piston length at, 40%, then 60%, 80%, 100% and back
(80%, 60%, 40%, 20%).
4 Verify the average flowrate for each piston position, calculate the hourly flow rate in
Kg/h and draw the calibration curve on a graph paper sheet, comparing the piston
length in % and the flowrate in Kg/h.

5.7 Pre-commissioning completion

The final step of the pre-commissioning phase is the "Wet run”: generic name of the test,
performed using the most appropriate fluids at the operating conditions of the plant.
Purpose of this test is the simulation of the process conditions and familiarization of plant
staff with plant operations. The test is executed as much as possible according to the start-
up instruction of the Operation Handbook, and the entire plant is checked with reference to
the P&I diagrams.
The simulation consists of:
1. Raw material in the sulphonation reactor circuit.
2. Exhaust gas unit in operation
3. Process air compression and dehumidification in operation
4. SO2-SO3 unit preheating.

The activities of this step are the following:

Adjustment and check of instruments
- Test of control valves, interlock system and alarm systems
- Check of mechanical installation and test of tightness
- Further checks of correct installation of safety valves, vents, valves and non-return
valves.
- Check of equipment pressure drop.
Test must be made on pumps, stirrers, compressors. turbines, etc.
If possible, the temperature of the heaters is raised to the normal operating value, after
which the flange bolts are tightened. All joints must be checked for leakage.
During the pre-commissioning period, the insulation, weather-proofing and painting of all
the equipment, pipe lines and instruments (as per specifications) must be completed,
inspected and approved.
 1E55-40-600 OPERATION HANDBOOK 45

5.8 Pre-commissioning procedures: WHAT IF

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 01: Mechanical Procedures (Pressure & Hydraulic test)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Priority
(Prevention/Protection)
R1 - Inform that the operation is being
Possible people Personal Protection executed
What can happen during the pressure and injuries due to objects Equipment (PPE)
1. 1 R2 - Guarantee the area isolation
hydraulic test execution? fall, impact and
leakage of fluid test Area isolation R3 - Guarantee the use of proper
personal protection equipment (PPE)
Possible people
What can happen if the test is not injuries due to
2. 3
executed? product/gas leakage
(toxic)
Damaged to
equipment R2 - Guarantee the area isolation
What can happen if the procedure has not
3. been executed properly (vent, bolt Possible people 3 R3 - Guarantee the use of proper
tightening, etc)? injuries personal protection equipment (PPE)
Restart the procedure
 1E55-40-600 OPERATION HANDBOOK 46

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 02: Mechanical Procedures (General activities)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
Possible people
What can happen during the general Personal Protection R1 - Inform that the operation is being
1. injuries due to objects 2
inspection of the plant conformity? Equipment (PPE) executed
fall and impact.
What can happen if is not executed the Possible problems
2.
general inspection of the plant conformity? during plant start-up
What can happen during remove all rust No major
3. preventives oils used to protect the consequence or
equipment? hazard
Possible fire with
What can happen if it is not removed all consequent people R2 - Guarantee the correct execution
Personal Protection
4. rust preventives oils used to protect the injuries 3 without the use of solvent and notify
Equipment (PPE)
equipment? when the execution is done
Damage of equipment
Possible damage to
R3 - See equipment technical
equipment
What can happen during remove all specification
Possible people Personal Protection
5. temporary supports, bracings or other 1 R4 - Use proper devices to remove all
injuries due to Equipment (PPE)
foreign objects? temporary supports, bracings or other
improper use of
foreign objects
devices
Damage of equipment
Possible people R5 - Create a checklist in order to control
What can happen if it is not removed all
injuries due to object Personal Protection the correct plant set-up, based on the
6. temporary supports, bracings or other 3
fall and impact Equipment (PPE) Pre-commissioning & commissioning
foreign objects?
checklist
Possible leakage of
toxic gas
 1E55-40-600 OPERATION HANDBOOK 47

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 02: Mechanical Procedures (General activities)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
What can happen if it is not used the
7. Damage of equipment
proper lubrificant or if it is not added?
Possible damage to
R3 - See equipment technical
What can happen during the installation or equipment
specification
verification of mechanical seals, Possible people Personal Protection
8. 1 R4 - Use proper devices to remove all
permanent packing and accessories injuries due to Equipment (PPE)
where required? temporary supports, bracings or other
improper use of
foreign objects
devices
Damage of equipment
What can happen if it is not installed /
9. verified mechanical seals, permanent Possible people
packing and accessories where required? injuries, due to
leakage
R1 - Inform that the operation is being
executed
R6 - Uncoupling the motor from the
machine when perform the test, if
Area isolation
What can happen during the motor possible/required
10. Damage of equipment Personal Protection 1
rotation control? R7 - Before proceed the check motor
Equipment (PPE)
rotation, be sure the proper terminal
connection of the motor
R8 - Verify the supplier documentation
regarding the rotation direction
 1E55-40-600 OPERATION HANDBOOK 48

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 02: Mechanical Procedures (General activities)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
Damage of equipment
What can happen if it is not checked Possible people
11. phase sequence and polarity (motor injuries due to
rotation)? electrical shock or
object impact
R1 - Inform that the operation is being
executed
R9 - Identify with locks and labels that the
Possible people Personal Protection
12. What can happen during cold alignment? circuit to be tested is not energized
injuries Equipment (PPE)
R10 - Guarantee that the circuit will not
be accidentally or intentionally energized
(locks, labels, etc)
Damage of equipment
During the plant
What can happen if the cold alignment is operation, possible
13.
not executed? damage of equipment
with possible lost of
production

14. What can happen during field test? Refer to Mechanical

procedure (pressure
What can happen If it is not executed field and hydraulic test)
15.
test?
 1E55-40-600 OPERATION HANDBOOK 49

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 02: Mechanical Procedures (General activities)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
R1 - Inform that the operation is being
Possible people executed
What can happen during the removal of all
injuries with steam and Personal Protection
16. steam traps and flush heating lines and 3 R11 - Guarantee the area isolation
possible impact with Equipment (PPE)
coils with steam?
“dirty” inside the line R12 - Use of PPE specific for noisy
operation
Possible damage of
equipment
What can happen if it is not removed all During the plant
17. steam traps and flush heating lines and operation, possible
coils with steam? damage of equipment
with possible lost of
production
 1E55-40-600 OPERATION HANDBOOK 50

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 03: Mechanical Procedures (Flushing activities / Leak test / Filling activities)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)

Possible leakage of R1 - Inform that the operation is being

water Area isolation executed
What can happen during flushing with
1. Possible people Personal Protection 1 R2 - Guarantee the area isolation
water?
injuries due to slippery Equipment (PPE) R3 - Guarantee the use of proper
floor. personal protection equipment (PPE)
Possible damage of
equipment

What can happen if flushing is not During the plant

2. operation, possible
executed?
damage of equipment
with possible lost of
production
R1 - Inform that the operation is being
Possible leakage of air executed
Area isolation
3. What can happen during flushing with air? Possible people 1 R2 - Guarantee the area isolation
Personal Protection
injuries due to object
Equipment (PPE) R3 - Guarantee the use of proper
fall and impact
personal protection equipment (PPE)
Possible damage of
equipment

What can happen if flushing is not During the plant

4. operation, possible
executed?
damage of equipment
with possible lost of
production
 1E55-40-600 OPERATION HANDBOOK 51

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 03: Mechanical Procedures (Flushing activities / Leak test / Filling activities)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
R1 - Inform that the operation is being
executed
Possible people Area isolation
What can happen during flushing of R2 - Guarantee the area isolation
5. injuries due to toxic Personal Protection 3
catalyst tower?
particles emission Equipment (PPE) R4 - Guarantee the use of proper
personal protection equipment (PPE) and
safety mask for particulate material
Possible damage of
equipment

What can happen if flushing of catalyst During the plant

6. operation, possible
tower is not executed?
damage of equipment
with possible lost of
production
R1 - Inform that the operation is being
Possible people Personal Protection executed
What can happen during leak test of jacket injuries due to objects Equipment (PPE)
7. 1 R2 - Guarantee the area isolation
lines/equipments? fall, impact and
leakage of product Area isolation R3 - Guarantee the use of proper
personal protection equipment (PPE)
Possible damage of
equipment

What can happen if the leak test is not During the plant
8. operation, possible
executed?
damage of equipment
with possible lost of
production
 1E55-40-600 OPERATION HANDBOOK 52

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 03: Mechanical Procedures (Flushing activities / Leak test / Filling activities)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
R1 - Inform that the operation is being
executed
Possible people
injuries due to particles R2 - Guarantee the area isolation
Area isolation
What can happen during the filling of silica inhalation R4 - Guarantee the use of proper
9. Personal Protection 2
gel or activated alumina? Possible people personal protection equipment (PPE) and
Equipment (PPE)
injuries due to high safety mask for particulate material
weight of the drum
R5 - Guarantee the use of forklift or
similar
What can happen if it is not executed the Plant can not be
10.
filling with silica gel or activated alumina? startup
R1 - Inform that the operation is being
executed
Possible people
injuries due to toxic R2 - Guarantee the area isolation
Area isolation
What can happen during the filling of particles inhalation
11. 3 R4 - Guarantee the use of proper
vanadium pentoxide? Personal Protection
Possible people personal protection equipment (PPE) and
Equipment (PPE)
injuries due to high safety mask for particulate material
weight of the drum
R5 - Guarantee the use of forklift or
similar
What can happen if it is not executed the Plant can not be
12.
filling with vanadium pentoxide? startup
 1E55-40-600 OPERATION HANDBOOK 53

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Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 04: Mechanical Procedures (Air Drying Unit)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)

Silica gel charging – See filling activities

1.
(item 9 and 10)

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 05: Mechanical Procedures (Sulphur Furnace Curing)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
R1 - Inform that the operation is being
Personal Protection executed
People injuries due to Equipment (PPE)
1. What can happen during the curing? 3 R2 - Guarantee the area isolation
high temperature
Area isolation R3 - Guarantee the use of proper
personal protection equipment (PPE)
During plant operation,
What can happen if it is not performed the
2. possible damage to
curing?
equipment
 1E55-40-600 OPERATION HANDBOOK 54

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Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 06: Mechanical Procedures (SO2 / SO3 Converter Column)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)

See filling activities - Vanadium pentoxide

1.
(item 11 and 12)
 1E55-40-600 OPERATION HANDBOOK 55

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Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 07: Mechanical Procedures (Film Reactor)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
Possible people
What can happen during reactor verticality Personal Protection R1 - Inform that the operation is being
1. injuries due to objects 2
check? Equipment (PPE) executed
fall and impacts.
What can happen if it is not checked the During plant operation,
2.
reactor verticality? production problems

3. Line flushing – see flushing activities

R1 - Inform that the operation is being

Personal Protection executed
Possible people
What can happen during reactor Equipment (PPE)
4. injuries due to objects 2 R2 - Guarantee the area isolation
calibration?
fall and impacts. Area isolation R3 - Guarantee the use of proper
personal protection equipment (PPE)
What can happen if it is not executed the Plant can not be
5.
reactor calibration? startup
R1 - Inform that the operation is being
Personal Protection executed
Possible people
What can happen during reactor tubes Equipment (PPE)
6. injuries due to objects 2 R2 - Guarantee the area isolation
blinding?
fall and impacts. Area isolation R3 - Guarantee the use of proper
personal protection equipment (PPE)
 1E55-40-600 OPERATION HANDBOOK 56

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Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 08: Mechanical Procedures (ESP)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
Possible people
What can happen during ESP verticality Personal Protection R1 - Inform that the operation is being
1. injuries due to objects 2
check? Equipment (PPE) executed
fall and impacts.
What can happen if it is not checked the During plant operation,
2.
ESP verticality? ESP mal function
Possible people
Personal Protection R1 - Inform that the operation is being
What can happen during ESP assembling injuries
3. Equipment (PPE) 3 executed
(insulators)? Possible damage to
Area isolation R2 - Guarantee the area isolation
equipment
R1 - Inform that the operation is being
executed
Possible damage to
equipment R2 - Guarantee the area isolation
Personal Protection
What can happen during ESP assembling Possible people Equipment (PPE) R3 - See equipment technical
4. 3
(tube bundles) injuries due to specification
Area isolation
improper use of
devices R4 - Use proper devices to remove all
temporary supports, bracings or other
foreign objects
What can happen if it is not checked the During plant operation,
5.
tube bundles leveling? ESP mal function
 1E55-40-600 OPERATION HANDBOOK 57

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 08: Mechanical Procedures (ESP)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
R1 - Inform that the operation is being
executed
Possible damage to
equipment R2 - Guarantee the area isolation
Personal Protection
What can happen during ESP assembling Possible people Equipment (PPE) R3 - See equipment technical
6. 3
(high-voltage electrode) injuries due to specification
Area isolation
improper use of
devices R4 - Use proper devices to remove all
temporary supports, bracings or other
foreign objects
What can happen if it is not centered the During plant operation,
7.
high voltage electrode ESP mal function
 1E55-40-600 OPERATION HANDBOOK 58

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Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 09: Mechanical Procedures (Metering Proportioning Pumps)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
Possible people
What can happen during pump injuries due to leakage Personal Protection R1 - Inform that the operation is being
1. 3
calibration? of products / raw Equipment (PPE) executed
material
During plant operation,
What can happen if it is not executed the
2. possible lost of
pump calibration?
production
 1E55-40-600 OPERATION HANDBOOK 59

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Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 10: Electrical Procedures (Electrical Power and Lighting System) Revision: 0

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
R1 - Verify that the circuit is not
energized

Possible people R2 - Inform that the test is being

injuries executed
What can happen during the insulation Area isolation
Damaged the R3 - Identify with locks and labels that the
1. test of wiring (if the line to be tested is Personal Protection 3
instrument in use to circuit to be tested is not energized
already energized)? Equipment (PPE)
the test R4 - Guarantee that the circuit will not be
(megohmmeter) accidentally or intentionally energized
(locks, labels, etc)
R5 - Guarantee the area isolation
Damaged to
equipment, cables,
terminals, electrical
board.
What can happen if it is not performed
2.
insulation test of wiring? Possible fire with
people injuries.
Possible electrical
shock.
Possible people
Area isolation R2 - Inform that the test is being
What can happen during grounding injuries
3. 3 executed
system test? Personal Protection
Possible electrical
Equipment (PPE) R5 - Guarantee the area isolation
shock
 1E55-40-600 OPERATION HANDBOOK 60

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 10: Electrical Procedures (Electrical Power and Lighting System) Revision: 0

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
Possible people
injuries
Possible electrical
shock

What can happen if it is not Performed Possible failure of

4. control system,
grounding system tests?
electrical equipment,
instrumentation with
consequent possible
damaged during future
plant operation and
loss of production
R3 - Identify with locks and labels that the
circuit to be tested is not energized
R4 - Guarantee that the circuit will not be
accidentally or intentionally energized
(locks, labels, etc)
R6 - Inform that the operation is being
Area isolation executed
What can happen during check phase Damaged of
5. Personal Protection 1 R7 - Uncoupling the motor from the
sequence and polarity? equipment
Equipment (PPE) machine when perform the test, if
possible / required
R8 - Before proceed the check motor
rotation, be sure the proper terminal
connection of the motor.
R9 - Verify the supplier documentation
regarding the rotation direction
 1E55-40-600 OPERATION HANDBOOK 61

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 10: Electrical Procedures (Electrical Power and Lighting System) Revision: 0

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
Damaged of
equipment
What can happen if it is not checked Possible people
6.
phase sequence and polarity? injuries due to
electrical shock or
object impact
Possible people
What can happen during the installation of injuries Personal Protection R6 - Inform that the operation is being
7. 1
emergency power systems (UPS)? Possible electrical Equipment (PPE) executed
shock
During the plant
What can happen if it is not checked the
operation, unexpected
8. installation of emergency power systems
shutdown in case of
(UPS)?
electrical failure.
Possible people
What can happen during the installation of injuries Personal Protection R6 - Inform that the operation is being
9. 1
emergency power systems (EG)? Possible electrical Equipment (PPE) executed
shock
During the plant
operation, unexpected
What can happen if it is not checked the shutdown in case of
10. installation of emergency power systems electrical failure.
(EG)? Possible wrong
rotation of all the
motors.
 1E55-40-600 OPERATION HANDBOOK 62

What if

Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 10: Electrical Procedures (Electrical Power and Lighting System) Revision: 0

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
Possible people
What can happen during the illumination Personal Protection R6 - Inform that the operation is being
11. injuries due to objects 2
system check? Equipment (PPE) executed
fall and impact.
Possible people R10 - Notify the customer and/or the
What can happen if the illumination injuries project manager the situation
12. 3
system is not adequate? Impossible operation R11 - Guarantee the proper illumination
of the plant system in the plant
Possible people
What can happen during the check of all Personal Protection R6 - Inform that the operation is being
13. injuries due to objects 2
control circuit? Equipment (PPE) executed
fall and impact.
Possible people
injuries
What can happen if it is not checked all
14. Damaged of
control circuits for proper operation?
equipment
Loss of raw material
 1E55-40-600 OPERATION HANDBOOK 63

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Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 11: Electrical Procedures (Instrument System)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
R1 - Inform that the operation is being
Possible people executed
What can happen during instruments pre Personal Protection
1. injuries due to objects 2
inspection? Equipment (PPE) R2 - Check instrument TAG
fall and impact.
R3 - Check the supplier documentation
What can happen if it is not executed the Possible damaged to
2.
instruments pre inspection? instrumentation
Possible people
What can happen during instruments field Personal Protection R1 - Inform that the operation is being
3. injuries due to objects 2
calibration? Equipment (PPE) executed
fall and impact.
Wrong indication of
What can happen if it is not executed the instruments, with
4.
instruments field calibration? consequence in the
process

What can happen during fully pressurize Possible people R1 - Inform that the operation is being
Personal Protection executed
5. and energize the transmitting and control injuries due to objects 2
Equipment (PPE)
signal system? fall and impact. R4 - Use of safety glasses if required
What can happen if it not executed the
During the plant
control mode settings and other
6. operation, process
adjustment to systems for automatic
disturbance can occur
operation of equipment?
Possible people
What can happen during the process lead Personal Protection R5 - Guarantee the use of proper devices
7. injuries due to use of 2
piping check for tightness? Equipment (PPE) if required.
improper devices
 1E55-40-600 OPERATION HANDBOOK 64

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Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 11: Electrical Procedures (Instrument System)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
During plant operation,
possible leakage of
gas (SO2, SO3) and
What can happen if it is not checked liquid (NaOH, Sulfuric
8.
process lead piping for tightness? acid, oleum)
Possible people
injuries
Possible people
injuries
What can happen during the relief valves Damaged to
9. Area isolation 3 R6 - Guarantee the area isolation
test? equipment, lines.
Leakage of dangerous
product
Possible people
injuries
Damaged to
What can happen if it is not tested all relief
10. equipment, lines.
valves?
During plant operation,
possible leakage of
dangerous product
 1E55-40-600 OPERATION HANDBOOK 65

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Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 12: Electrical Procedures (Pre Heater / ESP / Boiler)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
R1 - Inform that the operation is being
executed
R2 - Guarantee the area isolation
Possible risk of fire or Personal Protection R3 - Guarantee the use of proper
What can happen during the leakage test explosion, with Equipment (PPE)
1. 3 personal protection equipment (PPE)
in the gas line (Pre heater)? consequent people
injuries Area isolation R4 - Follow the burner operation
handbook
R5 - Guarantee patent person for the
procedure, when required
At plant start-up,
possible risk of fire or
What can happen if the leakage test in the
2. explosion, with
gas line is not performed (Pre heater)?
consequent people
injuries
R2 - Guarantee the area isolation
R6 - Inform that the test is being
Possible people executed
injuries R7 - Verify that the circuit is not
What can happen during the cable Area isolation
Damaged the energized
3. isolation, grounding test and safety device Personal Protection 3
verification (ESP)? instrument in use to R8 - Identify with locks and labels that the
Equipment (PPE)
the test circuit to be tested is not energized
(megohmmeter)
R9 - Guarantee that the circuit will not be
accidentally or intentionally energized
(locks, labels, etc)
 1E55-40-600 OPERATION HANDBOOK 66

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Date: July 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 01: Pre- commissioning procedure Subsystem 12: Electrical Procedures (Pre Heater / ESP / Boiler)

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
At plant start-up,
What can happen if the cable isolation, possible risk of fire or
4. grounding test and safety device explosion, with
verification are not executed (ESP)? consequent people
injuries
R1 - Inform that the operation is being
executed
R2 - Guarantee the area isolation
Possible risk of fire or Personal Protection R3 - Guarantee the use of proper
What can happen during the leakage test explosion, with Equipment (PPE)
5. 3 personal protection equipment (PPE)
in the diesel oil/gas line (Boiler)? consequent people
injuries Area isolation R4 - Follow the burner operation
handbook
R5 - Guarantee patent person for the
procedure, when required
At plant start-up,
What can happen if the leakage test in the possible risk of fire or
6. diesel oil/gas line is not performed explosion, with
(Boiler)? consequent people
injuries
 1E55-40-600 OPERATION HANDBOOK 67

Severity Categories

Category Severity Safety Environment

5 Catastrophic Multiple fatalities Very serious groundwater / water course contamination
4 Major Single fatality Major loss of harmful or toxic liquid
3 Severe Multiple or severe injuries Some environmental damage
2 Significant Lost time accident Release of hazardous material offsite. Complaints
1 Minor Minor injury No offsite effect. Material contained

General Recommendation : use the Personal Protection Equipment (PPE) when required for the activity conform to the “ Safety Prescriptions for
Pre-commissioning, Commissioning and Start-up Activities”.
 1E55-40-600 OPERATION HANDBOOK 68

5.9 Pre-commissioning procedures: HAZARD IDENTIFICATION

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 01: Mechanical Procedures (Pressure & Hydraulic test) Revision: 0

Activity Hazard Cause Consequence Recommendations Observations Ref

Possible people
Pressure and Line to be prepared injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
hydraulic test and tested not Lack of floor and/or from height
using applicable standard or line instead of proper 1
preparation and reachable by the test dedicated platform
Preparation and test rolling safety ladders scaffolding
execution executors
can not be executed
 1E55-40-600 OPERATION HANDBOOK 69

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 02: Mechanical Procedures (General activities) Revision: 0

Activity Hazard Cause Consequence Recommendations Observations Ref

Remove all
temporary
supports, bracings
or other foreign
objects that were
installed in Possible people
Temporary support, injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
vessels, rotating
bracings and others Lack of floor and/or from height
equipment, using applicable standard or line instead of proper 1
are not reachable by dedicated platform
electrostatic Removal can not be rolling safety ladders scaffolding
the executors
precipitator or executed
other equipment to
prevent damage
during shipping,
storage and
erection
Mechanical seals, Possible people
Install mechanical injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
permanent packing
seals, permanent Lack of floor and/or from height
and accessories not using applicable standard or line instead of proper 2
packing and dedicated platform
reachable by the Installation can not rolling safety ladders scaffolding
accessories
executors be executed
 1E55-40-600 OPERATION HANDBOOK 70

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 02: Mechanical Procedures (General activities) Revision: 0

Activity Hazard Cause Consequence Recommendations Observations Ref

R1. Provide proper scaffolding

Check rotating
Possible people using applicable standard or
machinery for
correct direction of injuries due to fallen rolling safety ladders O1. It’s forbidden to use pipe
Motor not reachable Lack of floor and/or from height
rotation and for R2. Guarantee the area line instead of proper 3
by the test executor dedicated platform
freedom of moving Test can not be isolation scaffolding
parts before executed R3. Inform that the test is
connecting driver
being executed
R1. Provide proper scaffolding
Possible people using applicable standard or
injuries due to fallen rolling safety ladders O1. It’s forbidden to use pipe
Make shaft cold Motor not reachable Lack of floor and/or from height
R2. Guarantee the area line instead of proper 4
alignment by the executor dedicated platform
Alignment can not isolation scaffolding
be executed R3. Inform that the test is
being executed
 1E55-40-600 OPERATION HANDBOOK 71

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 03: Mechanical Procedures (Filling activities) Revision: 0

Activity Hazard Cause Consequence Recommendations Observations Ref.

Possible people
Manhole not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 1
dedicated platform
Filling of silica gel installator Filling can not be rolling safety ladders scaffolding
or activated executed
alumina
Possible people
Handling of injuries due to R2. Guarantee the use of
Heavy weight of drum 2
inventory handling heavy forklift or similar
drum
Possible people
Manhole not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 3
dedicated platform
installator Filling can not be rolling safety ladders scaffolding
Filling of vanadium
executed
pentoxide
Possible people
Handling of injuries due to R2. Guarantee the use of
Heavy weight of drum 4
inventory handling heavy forklift or similar
drum
 1E55-40-600 OPERATION HANDBOOK 72

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 03: Mechanical Procedures (Filling activities) Revision: 0

Activity Hazard Cause Consequence Recommendations Observations Ref.

Possible people
Manhole not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 5
dedicated platform
Filling of refractory installator Filling can not be rolling safety ladders scaffolding
material for executed
sulphur furnace
Possible people
Handling of injuries due to R2. Guarantee the use of
Heavy weight of drum 6
inventory handling heavy forklift or similar
drum
Possible people
Filling Packing injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Manhole not
material (pall Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 7
plastic rings) for dedicated platform
installator Filling can not be rolling safety ladders scaffolding
scrubber
executed
 1E55-40-600 OPERATION HANDBOOK 73

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 04: Mechanical Procedures (Air Drying Unit) Revision: 0

Activity Hazard Cause Consequence Recommendations Observations Ref.

Possible people
Manhole not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 1
dedicated platform
Filling of silica gel operator Filling can not be rolling safety ladders scaffolding
or activated executed
alumina
Possible people
Handling of injuries due to R2. Guarantee the use of
Heavy weight of drum 2
inventory handling heavy forklift or similar
drum
Possible people
Manhole not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 3
dedicated platform
operator Maintenance can rolling safety ladders scaffolding
Maintenance not be executed
Possible people
Handling of injuries due to R2. Guarantee the use of
Heavy weight of drum 4
inventory handling heavy forklift or similar
drum
 1E55-40-600 OPERATION HANDBOOK 74

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 05: Mechanical Procedures (Sulphur Furnace Curing) Revision: 0

Activity Hazard Cause Consequence Recommendation Observations Ref.

Possible people
Manhole not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 1
dedicated platform
Filling of refractory operator Filling can not be rolling safety ladders scaffolding
material for executed
sulphur furnace
Possible people
Handling of injuries due to R2. Guarantee the use of
Heavy weight of drum 2
inventory handling heavy forklift or similar
drum
 1E55-40-600 OPERATION HANDBOOK 75

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 06: Mechanical Procedures (SO2 / SO3 Converter Column) Revision: 0

Activity Hazard Cause Consequence Recommendation Observations Ref.

Possible people
Manhole not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 1
dedicated platform
operator Filling can not be rolling safety ladders scaffolding
Filling of vanadium
executed
pentoxide
Possible people
Handling of injuries due to R2. Guarantee the use of
Heavy weight of drum 2
inventory handling heavy forklift or similar
drum
Possible people
Manhole not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 3
dedicated platform
operator Maintenance can rolling safety ladders scaffolding
Maintenance not be executed
Possible people
Handling of injuries due to R2. Guarantee the use of
Heavy weight of drum 4
inventory handling heavy forklift or similar
drum
 1E55-40-600 OPERATION HANDBOOK 76

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 07: Mechanical Procedures (Film Reactor) Revision: 0

Activity Hazard Cause Consequence Recommendation Observations Ref.

Removal of bottom
cone and temporary Impossible to reach
R1. Provide proper scaffolding O1. It’s forbidden to use pipe
installation of Lack of floor and/or the proper elevation
Reactor calibration using applicable standard or line instead of proper 1
calibration tubes not dedicated platform Calibration can not
rolling safety ladders scaffolding
reachable by the be executed
operator
 1E55-40-600 OPERATION HANDBOOK 77

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 08: Mechanical Procedures (ESP) Revision: 0

Activity Hazard Cause Consequence Recommendation Observations Ref.

R1. Provide proper scaffolding

Possible people using applicable standard or
ESP assembling – Lack of access injuries due to fallen rolling safety ladders
Bottom manhole not from height
high-voltage platform to bottom R2. Before any operation in 1
accessible
electrode manhole Assembling can not ESP, refer to supplier
be executed handbook (Corners) for
electrical safety operation
R1. Provide proper scaffolding
Possible people using applicable standard or
Lack of access injuries due to fallen rolling safety ladders
Bottom manhole not from height
ESP Cleaning platform to bottom R2. Before any operation in 2
accessible
manhole Cleaning can not be ESP, refer to supplier
executed handbook (Corners) for
electrical safety operation
Possible people
Bottom manhole not Lack of access injuries due to fallen R1. Provide proper scaffolding
accessible platform to bottom from height using applicable standard or 3
ESP maintenance manhole rolling safety ladders
Maintenance can
(high voltage
not be executed
electrode
replacement) R2. Before any operation in
Possible people
Electrical power on ESP, refer to supplier
Human error injuries due to 4
ESP panel handbook (Corners) for
electrical shock
electrical safety operation
 1E55-40-600 OPERATION HANDBOOK 78

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 08: Mechanical Procedures (SO2 Scrubber Column) Revision: 0

Activity Hazard Cause Consequence Recommendation Observations Ref.

Possible people
Filling Packing injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Manhole not
material (pall Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 1
plastic rings) for dedicated platform
installator Filling can not be rolling safety ladders scaffolding
scrubber
executed
 1E55-40-600 OPERATION HANDBOOK 79

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 09: Electrical Procedures (Electrical Power and Lighting System) Revision: 0

Activity Hazard Cause Consequence Recommendations Observations Ref.

R1. Provide proper scaffolding

Possible people using applicable standard or
Insulation tests of injuries due to fallen rolling safety ladders
Motor or transformer O1. It’s forbidden to use pipe
motor windings Lack of floor and/or from height
not reachable by the R2. Guarantee the area line instead of proper 1
and of transformer dedicated platform
test executor Test can not be isolation scaffolding
windings
executed R3. Inform that the test is
being executed
R1 Provide proper scaffolding
Possible people using applicable standard or
Check phase injuries due to fallen rolling safety ladders O1. It’s forbidden to use pipe
Motor not reachable Lack of floor and/or from height
sequence and R2. Guarantee the area line instead of proper 2
by the test executor dedicated platform
polarity Test can not be isolation scaffolding
executed R3. Inform that the test is
being executed
 1E55-40-600 OPERATION HANDBOOK 80

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 10: Electrical Procedures (Instrument System) Revision: 0

Activity Hazard Cause Consequence Recommendations Observations Ref.

Possible people
Instrument not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Instrument Lack of floor and/or from height
reachable by the using applicable standard or line instead of proper 1
installation dedicated platform
installator Installation can not rolling safety ladders scaffolding
be executed
Possible people
Instrument not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Instrument Lack of floor and/or from height
reachable for using applicable standard or line instead of proper 2
calibration dedicated platform
calibration Calibration can not rolling safety ladders scaffolding
be executed
Possible people
Leak tests of injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Control circuits not Lack of floor and/or from height
pneumatic control using applicable standard or line instead of proper 3
reachable for the test dedicated platform
circuits Test can not be rolling safety ladders scaffolding
executed
Possible people
Check process injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Piping not reachable Lack of floor and/or from height
lead piping for using applicable standard or line instead of proper 4
for the check dedicated platform
tightness Check can not be rolling safety ladders scaffolding
executed
 1E55-40-600 OPERATION HANDBOOK 81

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 10: Electrical Procedures (Instrument System) Revision: 0

Activity Hazard Cause Consequence Recommendations Observations Ref.

Check
thermocouples for
proper joining of Possible people
wires, position of Thermocouples not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Lack of floor and/or from height
elements in wells, reachable for the using applicable standard or line instead of proper 5
dedicated platform
proper polarity and check Check can not be rolling safety ladders scaffolding
continuity of executed
receiving
instruments
Insulate, or
remove if
necessary, inline
components such Possible people
as control valves, Inline components injuries due to fallen
R1. Provide proper scaffolding O1. It’s forbidden to use pipe
positive not reachable for Lack of floor and/or from height
using applicable standard or line instead of proper 6
displacement removal and re- dedicated platform Removal and re-
rolling safety ladders scaffolding
meters, turbine installation installation can not
meters, etc., for be executed
pressure testing
and re-install
them.
 1E55-40-600 OPERATION HANDBOOK 82

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 01: Pre- commissioning Procedure Subsystem 10: Electrical Procedures (Instrument System) Revision: 0

Activity Hazard Cause Consequence Recommendations Observations Ref.

Possible people
Orifice plates not injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Check bores of Lack of floor and/or from height
reachable for the using applicable standard or line instead of proper 7
orifice plates dedicated platform
check Check can not be rolling safety ladders scaffolding
executed
 1E55-40-600 OPERATION HANDBOOK 83

6. Commissioning and start-up procedure

6.1 Procedures before plant start up

A) Overall philosophy

The steps involved in this operation are:

- Utilities
- Raw material circulation through the reactor
- Exhaust gas treatment
- Air drying and gas scrubbing start-up
- SO2/SO3 conversion column preheating
- Sulphonation start-up (involving also ageing)

The main operations involving in the start up are described here in after:

NOTE: For the explanation it was considered the start up of plant processing LAB;
therefore all data are referred to LAB operation. When processing other products, the
general procedures are similar, while some operating parameters may change. Make
reference to the "Material and thermal balance" under ANNEX 3.

WARNING!
Chemical risk can be caused by hazardous substances used in plant
operation.
Check substance MSDS for related risk, exposure limits and safety
measures to be undertaken in case of exposure.
Check the location of emergency shower.
Wear personal protective equipment during operation for residual risk (refer to
Safety prescription for pre-commissioning, commissioning and start-up activities)

WARNING!
Danger of burns and injuries due to thermal contact.
During the operation all non-concerned personnel has to be moved away
from the area of piping under test and kept at safety distance.
Do not touch lines during steaming.
Personnel operating in plant area must wear personal protective
equipment for residual risk (refer to Safety prescription for pre-
commissioning, commissioning and start-up activities)
 1E55-40-600 OPERATION HANDBOOK 84

6.2 Utilities start up

For plant start-up all utilities are considered to be available at Battery Limits, that are:

Electric power
Low/medium pressure steam
Raw materials
Cooling water system
Compressed air/instrument air
Steam should be fed to the sulphur system at least 8 hours before start-up.

Before the plant start-up, the operator will check the setting of the instruments, the status
of manual valves and he will prepare the routing of the product, according to the raw
material to be processed.

6.3 Raw material circulation start up

(Re: Dwg 1E55.10.005 - sheet 1)

Before starting the air drying system it is necessary to put the organic raw material into
recycle through the sulphonation reactor 16R1; this operation is carried out, in order to
remove immediately from the internal pipes any dust or moisture presence contained in
the process air.

Proceed as follows:

1. Assure a sufficient amount of raw material in the feeding tank (battery limits).
2. Feed the raw material from the tank farm to the top of reactor 16R1, by
opening all relevant valves on pipes DD-16004. Open inlet/outlet valves of
filter 16F4A (or 16F4B) and start the feed pump.
Fill the EMERGENCY VESSEL item 16V3 with raw material, by opening
KV16.4 and HV 16.2 (close FV 16.3) up to the low level alarm LAL 16.1
disappears. Then close valve KV 16.4, HV 16.2 and open FV 16.3 .
Fill the vessel 16V3 with compressed air by opening relevant manual feeding
valve; wait till the pressure alarm indication, item PAL16.1, switches off (the
alarm set point, 6 bar), then,
- close compressed air valve.
- open the manual valve HV16.2..
- Set the pneumatic valve FV16.3 to the service of FIC16.3 at 70%.
When the flow rate is constant, open the vent valve on the top of reactor (see
item T7 on reactor data sheet), in order to purge the entrained air from the
organic chamber; then close the vent valve.
3. Within few minutes the raw material will be collected in the bottom part of
16R1 (see the sight glass on pipe DS16017); open the recycle valve HV 16.7
and start pump 16P2.
4. Check the level on LIC16.1 on the control panel and when it indicates more
than 100%, stop the organic feeding pump.
5. Adjust the speed rotation of 16P2, in order to read on FT16.3/FT16.4 an
indicative flowrate of 2300 Kg/h.
 1E55-40-600 OPERATION HANDBOOK 85

6. Start cooling water pump 16P1 and set TIC 16.7 at 28°C. The cooling water
recycling through 16R1 will be regulated according to the plant operation, by
adjusting the manual valves sited on the reactor outlet.

At this stage, the raw material is circulating in a close loop inside the reactor as follows:
pump 16P2 - mass flowmeter FE16.4 - filter 16F4A or 16F4B - mass flowmeter FE16.3 -
reactor 16R1 – pump 16P2.

NOTE: if during the plant operation the pressure alarm PAL16.1 occur, due to leaks;
immediately re-fill the emergency vessel 16V3, in order to assure the correct
operation of the emergency sequence.

6.4 Refrigeration group start up

(Dwg 1E55.10.002)

Open the delivery and suction valves of glycol pump 11P2 and start it
The glycol solution must be available at the operating temperature before air drying
start-up. In order to speed up the plant pre-heating (see following chapters), the chiller
group (11RGl, 11P2,) can be started as soon as cooling water is available at the plant.

1) Open the delivery and suction valves of glycol pump 11P2 and start it
1) Open cooling water supply to chilling group 11RG1 (pipe WR11101).
2) Start refrigerating group 11RG1 (switch on the power on local panel KU11.1)
following indication included into relevant manual
3) Start glycol recycle pump 11P1
4) Put in auto mode TIC 11.3 with required set point ( 1°C)
5) Wait when the temperature on TIC 11.3 will be reset at set-point value.

6.5 Exhaust gas treatment start up

(Dwg 1E55.10.004)

The tower 14C1 is supposed to be filled with the sulphite solution. Operator will check it
during the routing around the plant before start-up. If not, the tower must be filled with
water and caustic.

When the 14C1 scrubber is ready for operation, proceed as follows:

1) Start 14P1 recirculation pump at required flow.

2) Set flow of dilution water on flowmeter FI14.1. To avoid foam formation inside the
column, do not feed process water to the scrubber during preheating of catalyst tower
(i.e.: when there is no sulfur flow do not feed make-up water to 14C1).
3) Put pH control loop AE/AIT/AIC 14.1 into automatic mode and set at pH=10-12. Open
manual valves on the caustic soda feed line.
 1E55-40-600 OPERATION HANDBOOK 86

Before ESP (item 14F1) start up it is necessary to feed hot air to the top insulators, in
order to dry them from moisture; proceed as follows:

4) Start fan 12K1 and feed purge air to ESP via pipes AZ14007 (check the right position
of delivery manual valves)
5) Feed low pressure steam to the jacket of the exchanger 14E1.
6) Adjust the air temperature at about 70°C on TI14.2, by trottling the steam valve.

It is very important , especially after a long shut-down period, to purge, for few minutes ,
the ESP, in order to remove eventual light gas (Hydrogen) formed from the dilution of the
sulphuric acid by the moisture entered into the ESP : open valve KV16.3

6.6 Air drying section start up

(Dwg. 1E55.10.002)

One of the silica gel towers should have been regenerated previously to the start up of the
plant and is supposed to be ready for operation.

1) Set PIC 16.1 into manual mode, output = 0.

2) Close SO3 valve KV 16.5
3) Close the interception valves on quench air line to third and fourth catalyst layer.
4) Set FIC 16.1 into manual mode and FV 16.1 open .
5) Set FIC 16.2 into manual and FV16.2 closed.
6) Start 11K1 and set output of PIC 16.1 = 20%.

Purge the ESP, according to the automatic sequence (see URS ); then:
open the SO3 valve KV 16.5 to reactor.
7) Switch on the power on the control panel KU14.1, to the service of 14F1.
8) Set the suitable voltage and amperage to the 14F1 control panel.
9) Open the pneumatic valve FV16.2.
10) Put into automatic mode FIC16.2 and set the flow rate at S.P. = 2900 Kg/h”; such a
flow rate corresponds to the SO2/air concentration of 7% by volume, taking into
consideration to start the sulphur feed at 50% of nominal capacity.
11) Put into automatic mode PIC16.1; adjust the set point at 0.35 bar, which is the design
pressure of gas at the inlet of 16F3 in normal conditions. Of course such a parameter is
not fixed and could be adjusted during plant operation.
12) Close pneumatic valve FV 16.1 ( FIC 16.1 output = 0)
13) When the air flow is constant, the pre-heating burner can be started.

At this stage the air sucked from outside is compressed and dehumidified by means of the
following units:

- Filter on the suction of 11K1 having the purpose to entrap dust and powder from
atmospheric air sucked from compressor 11K1;
- Compressor 11K1.
- Chiller unit 11RG1 having purpose to remove the compression heat, to remove the
humidity from the air and also to convey low temperature air to the dehumidifying
tower, thus favouring the absorption of the still entrained water in the silica gel. The
process air is cooled down to 5°C by means of glycol solution.
 1E55-40-600 OPERATION HANDBOOK 87

- Dehumidifying tower 11C1A/B, having purpose to reduce to very low values (dew point
-60°C approx.) the moisture content of the air fed to the plant. This reduces to
acceptable values the oleum quantity produced in the conversion unit, which depends
directly to the quantity of water contained in the air.

The dehumidified air out flowing silica gel tower 11C1 is fed to plant as follows:
- Sulfur combustion furnace 12H1.
- Conversion unit 12C1.
- Air coolers 12E5, 12E6,
- SO3 filter 16F3.
- Sulphonation reactor 16R1.
- Gas-liquid separator 16V4.
- Cyclon 16S1.
- Electrostatic precipitator 14F1.
- Scrubber 14C1.

6.6.1 SILICA GEL REEGNERATION PROCEDURE

As previously described, the process air drying is performed by means of two parallel silica
gel layers; one in operation and the other under regeneration.
The process air flow is diverted from one to the other in order to obtain at any time the
lowest air dew point.

The beds are designed to work for 24 hours at maximum process air flow; consequently
with lower air flow, the time between two regenerations can be increased proportionally.
However, normal operating practice is to regenerate the beds every 8 hours without
considering the air flow.

The automatic sequence is controlled by means of several timers and temperature

indicators displayed by TI11.11 and TI11.7. (The step by step automatic sequence is
described in the URS - Spc. 1E55-40-280).

The operator according to process air moisture content or to the time schedule will
proceed to the beds exchange; the automatic regeneration will proceed as follows
(assuming that lower bed is under operation and upper bed is ready for operation):

BED PRESSURIZATION.

 At first, the PLC open ON/OFF valve KV11.8, in order to compensate the pressure
inside the two beds (so that limitating the pressure drop in the plant). After expiring the
dedicated timer, close the ON/OFF valve KV11.8 .

BED DEPRESSURIZATION.

 Open valve KV11.1B and close KV11.1A; so that inverting the beds operation (lower
bed to regeneration and upper bed under operation).
 1E55-40-600 OPERATION HANDBOOK 88

 The PLC proceeds automatically to depressurize the unit by opening the ON/OFF
valves KV11.2 and KV 11.4; after the timer set expiring, open KV 11.5,close KV11.4,
open KV 11.7,open KV 11.12,open KV 11.11

HEATING PHASE.

 Start fan 11K2. At this point the operator has two possible options:

a If regeneration is carried out by steam (as during start up), suck atmospheric
air by opening relative valve (pipe AT11011); open 8 bar steam to 11E1 (pipe
VB11107); discharge condensate via the relevant steam traps (pipe
CB11112 – CB11108).
b During normal operation, it is possible to make use of hot air coming from
heat recovery system, so that avoiding any steam consumption. Open
relative valve (pipe AH 12031),open KV 11.09 , close KV 11.10 and close the
steam supply to 11E1.

At this stage the regeneration circuit is the following: atmospheric air (or hot air coming
from catalysis) enters through the valve KV11.7 and flows through the fan 11K2,
vessel 11V1 (11E1), ON/OFF valve KV11.10 ( or ON/OFF valve KV 11.09),valve
KV11.11, drier 11C1 (lower bed),valve KV11.2,valve KV11.5, discharge to atmosphere
(pipe AV110110).

Regulate the air flowrate, in order to read a temperature of 160°C. on silica gel bed
inlet (TI11.12). According to option previously described proceed as follows:

a maintaining steam valve completely open to 11E1, adjust air flowrate by

means of regulating manual valve (pipe AT11017).
b Adjust the regulating valve (pipe AH 21002) and, since the temperature of
hot air coming from the heat recovery system is higher than 160°C, dilute the
air flow by feeding fresh air via regulating valve (pipe AT11011).

A checking about the effected regeneration is made, by verifying the outlet

temperature of the regeneration air on the temperature indicator TI11.11. Heating
operation will last into approximately 6 hours.

When the regeneration is completed, the silica gel mass has a temperature quite near
to 145 - 150°C. It is necessary to cool the silica gel, before putting into normal
operation the regenerated bed, thus allowing it to absorb the moisture of the air
crossing it. The PLC wait until the heating phase dedicated timer expires; then:

COOLING PHASE.

 The PLC close valve KV11.7 (closed circuit position - cooling phase) close the
ON/OFF valve KV11.5 and open the ON/OFF valve KV 11.6.
 1E55-40-600 OPERATION HANDBOOK 89

This operation has the purpose to create a closed circuit as follows: the hot air
outflowing 11C1 is sent through valve KV11.2, valve KV11.6, fan 11K2, vessel 11V1
(11E1), ON/OFF valves KV11.10, ON/OFF valve KV11.11 and back to drier 11C1
(lower bed).

 The operator close steam feeding and open cooling water feeding to 11E1, by opening
relevant cock (pipe WR11109).

The air circulating in this closed circuit is cooled in the battery 11V1; therefore, the
heat is removed from the silica gel layer: The PLC wait until the air outlet temperature
decreases down to about 30°C (under control of dedicated timer).

 The "COOLING" sequence is ended by PLC or when the operator selects the following
change of bed, so that starting a new regeneration step for the upper bed.

6.7 Pre-heating burner start up

(Dwg 1E55.10.003)

Purpose of this step is to put the catalyst in the best operating conditions in order to get in
the minimum time the best SO2/SO3 conversion. Assuming that the process air is already
started proceed as follows:

- Check that air fan 12K1 is running and feed cooling air to combustion fan 12K2 via pipe
AZ12015.
- Start fan 12K2.
- Feed gas to the burner and start the burner from the local panel BKI 12.1
- While pre-heating air is flowing to heat exchanger 12E2, finely tune the gas/air rate to
the burner, in order to regulate the combustion.
- Regulate the pre-heating air flow, in order to increase temperature progressively up to
580-600°C (TI12.14A), so that getting faster the preheating cycle. Increase and
maintain the temperature on first layer inlet (TI.12.3) in the range 390 - 420°C.
- The temperature probe TI12.14A and TI12.2 are recorded on local control board and
on the PC; in case of high temperature, TISHH12.14B is enabled to stop the burner;
set according to requirements.

At this stage the air conveyed by the fan 12K1 is heated in the hot air generator 12H2 from
which passes in the exchanger 12E2, where it is cooled down to about 250°C, before
being discharged to the atmosphere.
The process air coming from the blower 11K1 is heated inside 12E2 and progressively
preheats the stages of the catalysis tower 12C1. Once the tower beds heating is quite
homogeneous and the 1st bed outlet temperature is 380°C (TI12.4), the plant is ready to
start SO3 production.

The conversion unit is ready to receive the sulphur.

 1E55-40-600 OPERATION HANDBOOK 90

6.8 Sulphur melting and dosing pump setting / start up

(Dwg 1E55.10..007 )

The plant is provided with two sulphur pumps, each one designed for plant capacity.
Proceed as follows:

- Sulfur melting vessel 25V1 is filled with molten sulfur.

- Check the steam pressure and temperature; check all the steam jackets to service of
the sulfur pipe system and the efficiency of steam traps.
- Open related valves inlet/outlet the sulphur filter 25F1 ( or 25F2)
- Open related valves on suction pipe of dosing pump 25P1 (or 25P2)
- Start the electrical igniter 12H3
- Start the motor of the sulfur pump 25P1 (or 25P2).
- Set the piston stroke at the required flowrate,(normally 50% of nominal plant capacity)
according to the flow chart of the pump.
- Set in automatic mode FIC25.1, acting on FZ25.1.(or FZ 25.2).
- Melted sulfur will be fed to furnace 12H1, via pump 25P1 (or 25P2) and igniter 12H3.

6.9 Electrical igniter 12H3 start up

(Dwg. 1E55.10.003)

When the preheating is accomplished and it is time to ignite the sulfur proceed as follows:

- Open the valve of the sight glass 12Y2 on the furnace 12H1.
- Switch on the electrical panel to service of 12H3.(KU 12.1)
- Press the ignition push button located on the panel; the solenoid valve KY 12.1 is
energized (open) and electrical resistance reaches operating temperature in few
minutes. Wait until the sulfur is entering into furnace (it is possible to see it by using a
flash light and looking into sight-glass); then, open the compressed air valve and adjust
the pressure on PICV12.2, in order to have about 1 bar pressure.

The liquid sulfur, coming into 12H1, falls on incandescent electrical heater and in
presence of air ignites. The operator will be able to see the ignited sulfur falling down in
the furnace from the sight glass located on the combustion air nozzle 12Y1

Adjust the sulfur flow at 50% approx. of nominal plant capacity; that means set the piston
stroke in order to feed about 150 Kg/h (on LAB base). Since process air flowrate was fixed
at about 2900 Kg/h (see chapter 6.6), the SO2/SO3 concentration is 7% by volume.

Once the sulfur is ignited, the operator, after 30 seconds, must close the air valve and turn
OFF immediately the electrical heater (that in any case will be shut off by a timer set at 10
minutes), in order to prevent damage to the resistance.

NOTE:It is strongly suggested to install the cock valve on the air pipe AS12102
immediately before the inlet to sulfur pipe. The steam feeding line VB25005J will
keep indirectly hot the pipe, so that avoiding any clogging due to sulphureous gases
presence.
 1E55-40-600 OPERATION HANDBOOK 91

The process air entering into the furnace 12H1 from the bottom, enters into contact with
the ignited sulfur in the upper part of the furnace; as a consequence, sulfur burns
completely, forming SO2.
Now, following the catalyst tower temperatures, sulfur and process air can be increased up
to nominal flow.

Troubleshooting

Under normal conditions the sulfur ignites immediately. In case of failure to ignite, the
causes could be the following:

1 Absence of instrument air

2 Absence of electrical power or failure of the heater
3 The sulfur does not reach the incandescent electrical heater.

Should the sulfur fall to ignite, stop immediately the sulfur feeding into furnace 12H1 and
check that all the components are working properly.

6.10 SO3 production start up

(Dwg. 1E55.10.003)

Assuming that the pre-heating phase has been carried out, sulfur dosing has been started
and ignition is regular, proceed as follows:

1 Wait until temperature at the outlet of sulfur burner reaches 150°C (TI12.1A) as
minimum.
2 Increase the gas flow up to nominal capacity that is 5600 Kg/h, acting on FIC16.2
(already in automatic mode); open the dilution air valve FV16.1 and set the nominal
capacity of 720 Kg/h, acting on FIC16.1 (put FIC16.1 in automatic mode).
3 Wait when the pressure on PIC 16.1 ( in auto mode) reaches again the set point value
4 Meanwhile increase the sulphur flow to the nominal value
5 Wait when the pressure on PIC16.1 and the flowrates on FIC16.1 ,FIC16.2 anf FIC
25.1 are stable,

Temperatures

During the starting phase the conversion degree is rather low, but the heat which develops
progressively increases the temperature inside the tower, causing an increase of the
reaction speed until reaching the steady conversion degree (98% minimum).
The catalysis tower 12C1 is subdivided into four sections, each one consisting of a catalyst
layer and of the spaces for the gas inlet and outlet.
Afterwards, it will be necessary to cool the gas stream coming out of the furnace 12H1 in
the heat exchanger, because after sulfur combustion the gas comes out of the furnace at a
temperature of 600 –650°C, since reaction is highly exothermic.
 1E55-40-600 OPERATION HANDBOOK 92

Proceed as follows.
1 The operator must keep the preheating burner ON and slowly turn it down, in order to
keep the temperature at the inlet of the first catalyst layer in the range 410 - 430°C
(TI12.2) at least.
2 Wait untill the temperature of gas outflowing the furnace (TI12.1A) reaches 450°C;
then, stop burner 12H2. Stop also the cooling air supply through the pipes AZ12006
and pipe AZ12016, by closing the relative valves; stop the fan 12K2.
3 Take under close control the temperature increase and progressively open cooling air
valves to exchangers 12E2 (pipes AZ12006-AZ12025), 12E3 (pipe AZ12009).
4 Open manual valve on quench air line of third and fourth stage to keep the temperature
TI12.7 and TI12.9 approx 440°C
5 During start-up, the conversion is low and therefore the amount of heat developed is
low; thus the operator should increase/decrease the flow of cooling air to the
exchangers, in order to keep the temperature as close as possible to the optimum.

NOTE:
Under steady conditions, the heat exchangers 12E2, 12E3 have to bring back the
temperature of the reaction gas to the optimum value at inlet of every catalyst layer.
On the other way, the air coolers 12E5, 12E6 lower progressively the gas temperature
after conversion, so that the gases reach the utilization at 50-60°C.

6 During the gas cooling, the small quantities of sulphuric acid, which formed owing to
small quantity of water present in the process air, condense. The obtained oleum
(being SO3 in excess as to the water) is discharged periodically through the pertinent
valves, then getting into the collecting pipes HS12020, HS12021. The mist separating
filter 16F3 prevent however oleum drops from being entrained towards the utilization.
The oleum is pushed to scrubber 14C1 by means of compressed air. Make reference
to the URS specification ,Doc 1E55.40.280 for detailed explanation of the automatic
sequence
7 The temperature indicated for the different sections of the catalysis tower are the most
suitable to obtain a good conversion efficiency of the catalyst for a long time. Higher
temperatures than indicated, would cause a shortening of the catalyst life. Lower
temperatures would cause a reduction of the conversion efficiency.

The following temperatures should be maintained under steady running conditions:

Instrument Temperature °C

TI 12.1A 620-660°C Furnace outlet 12H1

TI 12.3 415-430°C 1st stage inlet
TI 12.4 570-590°C 1st stage outlet
TI 12.5 435-445°C 2nd stage inlet
TI 12.6 460-480°C 2nd stage outlet
TI 12.7 435-445°C 3rd stage inlet
TI 12.8 440-445°C 3rd stage outlet
TI 12.9 420-430°C 4th stage inlet
TI 12.10 410-430°C 4th stage outlet
TI 12.11 180-190°C 1st SO3 cooler outlet
TI 12.12 50 – 70 °C 2nd SO3 cooler outlet
 1E55-40-600 OPERATION HANDBOOK 93

As already explained, on the outlet of furnace 12H1 the temperature indicator TI12.1A is
placed; in case temperature arises more than set value they will indicate it on the PC and
the switch alarm TISHH12.1B will shut down the sulfur feeding pumps.

The sulfur combustion takes place in the upper part of the furnace 12H1; the refractory
balls contained in the lower part are purposed to increase the contact area of sulfur with air
and let it burn without reaching the furnace bottom.

6.11 Sulphonic acid production start up

(Dwg. 1E55.10.005)

Assuming that all the setting of process parameters required were already defined on the
basis of the "material balance", start up of sulphonation can be started as soon as the
conversion degree has been increased up to operating values. Proceed as follows:

6.11.1 RAW MATERIALS/PRODUCT ROUTING

Before start up provide that

- Raw material is available at the battery limits (tank farm).
- Ageing unit is ready
- Product receiver tank is ready
- Feeding pump is ready to be started and all relative valves are open.
- Raw material was fed to the reactor and is into recycle on it on following circuit:

filter 16F4A or 16F4B;

mass flowmeter FE16.3;
reactor 16R1;
gas/liquid separator 16V4;
pump 16P2 (set LZ16.1 manually in order to read 2400 Kg/h);
mass flowmeter FE16.4;
pipe DS16018 , HV 16.7 open , pipe 16021.

6.11.2 SULPHONATION START UP SEQUENCE

When the SO2/SO3 conversion starts increasing, the sulphonic acid production can be
started; proceed as follows:

 Wait when the sulphonic acid density raises 0,900 Kg/l ( DI 16.4)
 start feeding the fresh raw material from feeding tank
 open off-spec valve to the cubitainer and close recycle valve HV 16.7;

Moreover:

 put into automatic LIC16.1 (set the level at S.P. = 50%);

 put into automatic FIC16.3 (set the flow at 10 15% more than nominal flowrate);
 1E55-40-600 OPERATION HANDBOOK 94

At this stage operator has to start analyzing the acid value of the product at reactor outlet.
The analysis of the acid product at reactor outlet must be continuously performed every 5-
6 minutes; and the raw material feed on FIC16.3 must be continuously adjusted
accordingly.

As soon the acid value detected is acceptable, deviate the product to the Ageing section,
therefore:

 open valve HV 16.8;

 close off-spec valve to the cubitainer.

The optimizing of the flowrate to the reactor will end within 20-30 minutes; during all this
time continuous analysis will be carried out, in order to keep under control the acid value of
product.

NOTE:
During normal operation the operators may refer also to the density DI16.4, that is strictly
referred to the acidity of product.
During start up take care not to trust to density indications, untill the temperature of the
product (TI16.4) is stabilized at about 48-50°C.

ENABLE the Emergency sequence ( see URS – doc 1E55.40.280) for detailed
explanation.

6.11.3 AGEING STABILIZING UNIT START-UP

When the ageing tank 16A1 is half full, start the stirrer. Wait until the product overflows
from 16A1, then, proceed as follows:

- put LIC16.2 into automatic mode and start pump 16P4;

- open cooling water to the jacket of 16A1 and set the control loop TIC16.11, according
to the required ageing temperature;
- feed stabilizing water to 16Y1;
- open valve on pipe DS16037 ( B.L. ) or DS16042 ( unit 17 ) in according with the
production plan;
- feed cooling water to 16E1, in order to cool the product down to 30°C approx (make
reference to temperature indicator TI16.13).

At this stage the ageing section is automatically controlled; sulphonic acid is sent to battery
limit or to unit 17, through ageing tank 16A1 and extraction pump 16P4.
Operator will only adjust the stabilizing water feed, according to the analisys results (H 2O
final content 0,5% max. as average) and the ageing temperature 3-5°C higher than
sulphonic acid temperature on the outlet of 16R1 (see temperature indicator TI16.2).
Since the average temperature on TI16.2 is 48°C, maintain TIC16.11 at 52°C approx.
 1E55-40-600 OPERATION HANDBOOK 95

6.12 Double step neutralization start up / shut down

(Dwg 1E55.10.006)

FIRST START UP

Before feeding the acid to the neutralizing loop, the circuit must be prepared as follows:

1 Fill the circuit by means of process water and caustic soda and start the gear pump
17P2 (low speed), in order to recirculate a solution having 6% approx. as free
alkalinity. Start also mixer 17MX1.
2 Put into operation the cooling circuit to the service of heat exchanger 17E1, by
starting pump 17P3 and feed direct steam via pipe VB17110, in order to pre-heat the
solution of the loop at the operating temperature, that means 55-60°C.
3 Start feeding the sulphonic acid coming from section 16 (pipe DS16042) into mixer
17MX1.
4 After few minutes, start feeding the process water and the caustic soda via pump
17P1 at the design stoichiometric flowrate (adjust the piston strokes of 17P1 heads).
5 Close the direct steam to the cooling system and set into automatic mode TIC17.10,
so that removing the heat developed from the exothermic reaction.
6 Within few minutes the pressure detected from PIC17.3 start rising; therefore, set
17P2 at high speed and set into automatic mode PIC17.3, acting on PV17.3.
7 At this stage the paste will be discharged via pipe AN-DN17004 to the second mixer
22MX1.
8 Start 22MX1 and open relevant valves, in order to discharge the paste into 07A1 or
07A2 (pipes AN22001, AN07001 and AN07002).
9 Check the pH of the solution, by putting into operation the pH-meters AIT17.1 and
AIT22.1.

The output of AIT17.1 is automatically controlled via AIC17.1, acting on the piston
head “D” of pump 17P1; the output of AIT22.1 is automatically controlled via
AIC22.1, acting on the piston stroke AY22.1 of buffer pump 22P1.

10 Start buffer pump 22P1.

11 Wait until the level inside 07A1 covers the stirrer; then, start the stirrer and put into
recycle the paste, by opening relative valves (pipes AN07003, AN07004, AN07005)
and starting the gear pump 07P1.

After homogenization and analysis control, the product inside 07A1 can be
transferred as follows:

directly to storage via pipe AN07009 (diluted product).

to the deareator 28D1, via pipe AN07008 (concentrated product).
 1E55-40-600 OPERATION HANDBOOK 96

SHUT DOWN

The neutralization section can be easily stopped, by simply switching off the motors of
17P1, 17MX1, 17P2, 22MX1, 22P1.
Before stopping the dosing pumps, provide to turn to zero the piston stroke.
The sulphonation dosing must be shut down in the meantime, in order to avoid the
settling of unstable acid product inside the loop. At the end, put PIC17.3 in manual
mode.
Of course, provide to get empty the finishing tanks 07A1/2.

If required for the next start up, the operator will drain the entire system and wash the
loop by means of process water; otherwise the unit can be started as it is.

START UP (Loop full)

The start up procedure is much easier when the loop was left full during the previous
plant shut down. In such a case, the neutralizing section is ready to receive the
sulphonic acid, therefore, proceed as follows:

- Start the cooling system via pump 17P3 and set TIC17.10 at proper
temperature.
- Start 17P2, 17MX1, 22MX1, 22P1.
- Start dosing pump 17P1 and set all the heads of pump at their operating
position.
- Feed the acid from the reactor.

6.13 SLES deareation unit start-up

(Dwg. 1E55.10.008)

Before the unit start up, the operator shall provide to put under vacuum the deareator, by
starting the vacuum pump 28P2; proceeding as follows:

- open related valve (pipe AV28004) and start vacuum pump 28P2; feed process
water to the pump liquid ring, via pipe WP28101;
- Start 28D1 rotating distributor
- feed the neutralized product coming from B.L.; the product is sprayed on the
rotating distributor to the service of 28D1, before collecting on the bottom of the
vessel;
- after few minutes, open the extraction pump 28P1 delivery valve (pipe AN28003 to
storage tank ) and start it.
- Put into operation the level control LIC28.1, acting on the speed variator of gear
pump 28P1 and transfer the finished product .
 1E55-40-600 OPERATION HANDBOOK 97

6.14 Commissioning and start-up procedures: WHAT IF

What if

Date: July / 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 02: Commissioning and Start-up Procedures Subsystem 13: Commissioning and Start-up Procedures

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
Possible people
injuries due to objects
What can happen during raw material Personal Protection R1 - Inform that the operation is being
1. fall, impact and 2
circulation start-up? Equipment (PPE) executed
leakage of raw
material
Possible people
What can happen during refrigeration injuries due to objects Personal Protection R1 - Inform that the operation is being
2. 1
group start-up? fall, impact and Equipment (PPE) executed
leakage of product
Possible people
What can happen during Exhaust Gas injuries due to objects Personal Protection R1 - Inform that the operation is being
3. 1
Treatment Start-up? fall, shock and leakage Equipment (PPE) executed
of product
Possible explosion of
hydrogen present in
Exhaust Gas Treatment Start-up – What
the ESP with R4 - Guarantee the properly purging
4. can happen if the ESP purging sequence 3
consequence for sequence execution.
is not carried out?
person near by the
ESP
Possible people
What can happen during air Drying section injuries due to objects Personal Protection R1 - Inform that the operation is being
5. 1
start-up? fall, impact and Equipment (PPE) executed
leakage of product
 1E55-40-600 OPERATION HANDBOOK 98

What if

Date: July / 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 02: Commissioning and Start-up Procedures Subsystem 13: Commissioning and Start-up Procedures

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
R1 - Inform that the operation is being
executed
Possible risk of fire or Area isolation R5 - Guarantee the area isolation
What can happen during pre heating explosion, with
6. Personal Protection 3 R6 - Follow the burner operation
burner start-up? consequent people
injuries Equipment (PPE) handbook
R3 - Guarantee patent person for the
procedure, when required
Possible people
What can happen during sulphur pumping injuries due to objects Personal Protection R1 - Inform that the operation is being
7. 1
setting/start-up fall, impact and Equipment (PPE) executed
leakage of product
Possible people
What can happen during electrical Igniter injuries due to objects Personal Protection R1 - Inform that the operation is being
8. 1
start-up? fall, impact and Equipment (PPE) executed
leakage of product
Leakage of SO2 due
What can happen if electrical igniter fail to to sulphur
9. operate and sulphur continue to enter in accumulation and late 3
the furnace? ignition that cause
tube melting
R1 - Inform that the operation is being
Possible people executed
What can happen during SO3 production Personal Protection
10. injuries due to leakage 3
start-up? Equipment (PPE) R7 - Guarantee the availability of safety
of SO2/SO3
mask
 1E55-40-600 OPERATION HANDBOOK 99

What if

Date: July / 2011

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600
Revision: 0

System 02: Commissioning and Start-up Procedures Subsystem 13: Commissioning and Start-up Procedures

Safeguards
Ref No What If Consequence/Hazard Severity Recommendation & Action Note
(Prevention/Protection)
Possible people
What can happen during sulphonic Acid injuries due to objects Personal Protection R1 - Inform that the operation is being
11. 1
Production start-up? fall, impact and Equipment (PPE) executed
leakage of product
Possible people
What can happen during ageing injuries due to objects Personal Protection R1 - Inform that the operation is being
12. 1
Stabilizing Group Start-up? fall, impact and Equipment (PPE) executed
leakage of product
Possible people
What can happen during neutralization Personal Protection R1 - Inform that the operation is being
13. injuries due to leakage 2
start-up? Equipment (PPE) executed
of NaOH on flanges

Severity Categories

Category Severity Safety Environment

5 Catastrophic Multiple fatalities Very serious groundwater / water course contamination
4 Major Single fatality Major loss of harmful or toxic liquid
3 Severe Multiple or severe injuries Some environmental damage
2 Significant Lost time accident Release of hazardous material offsite. Complaints
1 Minor Minor injury No offsite effect. Material contained

General Recommendation : use the Personal Protection Equipment (PPE) when required for the activity conform to the “ Safety Prescriptions for
Pre-commissioning, Commissioning and Start-up Activities”.
 1E55-40-600 OPERATION HANDBOOK 100

6.15 Commissioning and start-up procedures: HAZARD IDENTIFICATION

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 02: Commissioning and Start-up Procedures Subsystem 11: Commissioning and Start-up Procedures Revision: 0

Activity Hazard Cause Consequence Recommendation Observations Ref.

Possible people
Utilities start-up injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Possible valves
(cooling water, Lack of floor and/or from height
and/or instruments using applicable standard or line instead of proper 1
steam, tank farm, dedicated platform
not accessible Start-up can not be rolling safety ladders scaffolding
compressed air)
executed
Possible people
Possible valves injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Raw material Lack of floor and/or from height
and/or instruments using applicable standard or line instead of proper 2
start-up dedicated platform
not accessible Start-up can not be rolling safety ladders scaffolding
executed
Possible people
Possible valves injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Refrigeration Lack of floor and/or from height
and/or instruments using applicable standard or line instead of proper 3
group start-up dedicated platform
not accessible Start-up can not be rolling safety ladders scaffolding
executed
Possible people
Possible valves injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Exhaust gas Lack of floor and/or from height
and/or instruments using applicable standard or line instead of proper 4
treatment start-up dedicated platform
not accessible Start-up can not be rolling safety ladders scaffolding
executed
 1E55-40-600 OPERATION HANDBOOK 101

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 02: Commissioning and Start-up Procedures Subsystem 11: Commissioning and Start-up Procedures Revision: 0

Activity Hazard Cause Consequence Recommendation Observations Ref.

Possible people
Possible valves injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Air drying section Lack of floor and/or from height
and/or instruments using applicable standard or line instead of proper 5
start-up dedicated platform
not accessible Start-up can not be rolling safety ladders scaffolding
executed
Possible people
Possible valves injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Pre heating burner Lack of floor and/or from height
and/or instruments using applicable standard or line instead of proper 6
start-up dedicated platform
not accessible Start-up can not be rolling safety ladders scaffolding
executed
Possible people
Possible valves injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
SO3 production Lack of floor and/or from height
and/or instruments using applicable standard or line instead of proper 7
start-up dedicated platform
not accessible Start-up can not be rolling safety ladders scaffolding
executed
Possible people
Sulphonic Acid Possible valves injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Lack of floor and/or from height
Production start- and/or instruments using applicable standard or line instead of proper 8
dedicated platform
up not accessible Start-up can not be rolling safety ladders scaffolding
executed
 1E55-40-600 OPERATION HANDBOOK 102

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E55-40-600 Date: July 2011

System 02: Commissioning and Start-up Procedures Subsystem 11: Commissioning and Start-up Procedures Revision: 0

Activity Hazard Cause Consequence Recommendation Observations Ref.

Possible people
Possible valves injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Neutralization Lack of floor and/or from height
and/or instruments using applicable standard or line instead of proper 9
start-up dedicated platform
not accessible Start-up can not be rolling safety ladders scaffolding
executed
 1E55-40-600 OPERATION HANDBOOK 103

Hazard Identification

Facility: Arma Soap Project - Sulphurex Plant Reference: Operation Handbook 1E52-40-600 Date: July 2011

System 03: Shutdown Procedure Subsystem 12: Shutdown Procedure Revision: 0

Activity Hazard Cause Consequence Recommendation Observations Ref.

Possible people
Possible valves injuries due to fallen R1. Provide proper scaffolding O1. It’s forbidden to use pipe
Shutdown Lack of floor and/or from height
and/or instruments using applicable standard or line instead of proper 1
activities dedicated platform
not accessible Shutdown can not rolling safety ladders scaffolding
be executed
 1E55-40-600 OPERATION HANDBOOK 104

7. Steady running condition

When the film sulphonation plants is steady running, the operator, expecially during the
first hours of operation, will have the task to take under deep control every part and
instrument of the plants.

It is quite important to verify continuously and carefully the running conditions of the plant,
in order to be able to detect immediately any sudden variation of the running parameters.

7.1 Oleum circuit

One time for shift, provide to discharge oleum from the bottom of coolers 12E5, 12E6,
12E7; and of the SO3 filter 16F3 therefore:

 Keep slightly opened the draining valves under 12E5, 12E6 and 16F3; the oleum
eventually present will be collected in the holding line.
 Activate the automatic draining sequence (make reference to the URS document –
1E55-40-280). The oleum will be sent into the scrubber, by means of compressed air.

During steady running conditions, adjust the timers to the service of automatic
sequence and adjust the air pressure on PICV12.1 (less than 1 bar).

WARNING!
Chemical risk can be caused by oleum.
Check substance MSDS for related risk, exposure limits and safety
measures to be undertaken in case of exposure.
Check the location of emergency shower.
Wear personal protective equipment during operation for residual risk (refer to
MSDS and to doc. 1D17-40-xxx – Safety prescription for pre-commissioning,
commissioning and start-up activities)

7.2 Operating log sheet

Prepare as soon as possible an OPERATING LOG SHEET, in order to report all the main
operating data of the plant, confined either to each operator’s duties or to the physical
division of the plant. All essential data should be recorded at least every two hours.

7.3 Analysis
Provide to carry out periodical complete analysis of the product, at least every two hours.

7.4 Reports
At a minimum of once a month, the supervisor or plant engineer should take a detailed
pressure and temperature survey throughout the plant at all points where connections
have been provided. These readings should be carefully studied and compared with
pressure/temperature trends and with design set points.
 1E55-40-600 OPERATION HANDBOOK 105

The survey report should contain all operating data collected on the daily report, all
additional temperatures and pressures throughout the plant, total production rate,
equivalent SO2 gas concentration, conversion efficiency, setting of gas by pass valves,
etc. All data should be obtained within a short period of time to give a true simultaneous
picture of plant operation. Also listed should be any shutdowns, major repairs, unusual
operating difficulties, rate changes, etc.

7.5 Pressure drops

Check as soon as possible the pressure drop of the plant at all the main stacks of
columns; detailed plant records of catalyst beds of conversion tower, packing,
sulphonation reactor, filters and packing on the scrubber, shall be periodically carried out
and noted, in order to easily detect possible problems arising on the gas circuit lines.

CATALYST
The efficiency of the catalyst can be seriously impaired, if the gas contains excessive
quantities of dust or acid mist. Mist can be produced by steam leaking into the sulfur or by
low efficiency of the drying tower. The moisture introduced from either of these sources
reacts with the small quantity of SO3, which will be present even before the gas enters the
converter, and forms minute droplets of H2SO4. The H2SO4 droplets will be absorbed by
the catalyst rings, reducing their efficiency, and, if the conditions are allowed to persist,
until disintegration takes place, causing partial “blinding” of the bed and high pressure
drop. Dust can be carried out in the system, when burning sulfur with high ash content or
from an improper operation of inlet air filter.
If the conversion efficiency falls off for a reason other than poor temperature control or
overload, and particularly if the decline is accompanied by an increase in the pressure
drop across a catalyst pass, then the catalyst should be examined and, if necessary,
screened to carefully remove dust and replaced in the converter
(see Spc. SB-PRO-C0001) .

7.6 Off-spec recovery

The off-spec material ( LAB partially sulphonated),collected into the cubitainer during
the plant start-up/shut-down phases, can be recovered dosing it ,by means the
proportioning pump 16P3, to the static mixer 16MX1.
The addition amount can be determine, starting from 2% of the raw material flow rate
and increasing it up to max 10%, in such away to avoid any negative effect on the
product out flowing from reactor ( i.e.: colour increasing, F.O. increasing, etc.)

7.7 E.S.P. purging sequence

The interlock between 11K1 and 14F1 must be by-passed to ensure that 14F1 will be
purged before being energized for a time long enough to get rid of any trace of hydrogen
that could be occasionally produced by carbon steel corrosion. The sequence will be
started by operator pushing a button located on the relevant video page, when purging is
performed 14F1 on video page will change colour.
For the sequence, make reference to the URS document – 1E55-40-280.
1E55-40-600 OPERATION HANDBOOK 106

8. Plant shut down

1. Disable the EMERGENCY SEQUENCE.

2. Stop sulphur pump 25P1 or 25P2. Wait untill the density detected on DT16.4
decreases, then, deviate the acid flowrate to the cubitainer OFF-SPECS

3. Stop the stabilizing water feed to 16Y1. Discharge the ageing unit into the LABS
tank. Wait untill the density decreases down to 0,900 Kg/cm3 on DT16.4, then, put
into recycle the raw material on the reactor.

4. Continue to flush the system for almost 30 minutes; purpose of flushing is double:

 Cool down the temperature of the conversion unit and wait untill the furnace
12H1 outlet temperature decreases lower than 200°C (see TI12.1A); in fact,
even if sulfur is stopped, the heat released from the concrete walls can
cause a strong increase of temperature (over allowed design basis).
 Push almost all the SO2/SO3 from the conversion unit to the reactor, so that
getting easier the next start up.

5. At the end stop the blowing section as follows:

Put PIC 16.1 in manual mode with output = 0 and stop blower 11K1 ; stop
refrigerating group 11RG1.
Close KV16.5 .
Decrease to zero the voltage and amperage on the ESP 14F1 control panel and
switch off the power on control panel KU14.1.
Stop cooling fan 12K1 (close related valves).
Close steam to 14E1.
Stop the exhaust gas scrubbing section (close NaOH feeding, stop the water
dilution valve, stop the recirculation pump 14P1);
stop the raw material recirculation on 16R1;
Stop cooling water pump 16P1.
 1E55-40-600 OPERATION HANDBOOK 107

8.1 Raw material change over and capacity variation

INTRODUCTION

Basically in case of LAE processing, the plant start-up and shut-down are
carried over previous change-over with LAB
There are two change over procedures:

1 Shut down of the sulphonation unit.

2 In line change over.

The first procedure is the most flexible and safe, but involves a certain loss of
production due to the time required to shut down and re-start the plant. Since it
is almost clear, it will be not more long discussed in this chapter.

In line change over is faster but involves the production of a certain amount of
mixed product; acceptance of such a procedure depends on various factors,
that mainly are raw materials compatibility, product specification, production
schedule.
In line change over procedure is best applicable when raw materials are similar
(for example when it involves two ethoxylated alcohols) and when there is not
need to change the paste concentration in the neutralizing unit.

The most critical parameters involved in such operation are:

raw material switch over: the operator must manage the switch over of the raw
materials taking care to maintain an excess of organic, in order to avoid
oversulphonation with consequent degradation of the product inside reactor. At
the same time the operator must take care not to produce big amounts of OFF-
specs. The synchronization of all the operations is a key factor to carry out the
change over safely and in a short time.

START-UP CHANGE OVER

Once the neutralizing unit is ready, proceed as follows:

1 Switch into manual the mole ratio (if in operation) and DISABLE THE
EMERGENCY SEQUENCE on 16R1.

2 Decrease the sulfur flow to LAE process nominal capacity.

3 Adjust the SO3 gas flow at the new operating set point

4 Increase the dilution air up to the new operating set point; variation on the
SO3 and air gas flows must be carry out with care, avoiding big variations on
the pressure of the circuit.

5 Decrease gradually the raw material flowrate, in order to maintain the

stechiometric rate with the SO3 feeding . Keep under control the density
variations on DI16.4.
 1E55-40-600 OPERATION HANDBOOK 108

6 During this period (around 30 minutes), the conversion degree could

decrease due to catalysis temperatures variations; that means it is advisable
to take under deep control the acid value of product outflowing 16R1, untill
all parameters are stable.

7 When the operating parameters are stabilized in the plant, it is possible to

change the raw material feed to the reactor. Proceed as follows:

- Since the stoichiometric ratios (related to LAE) are quite different, at

beginning it is strongly suggested to set FIC16.3 at a flowrate higher
than nominal to avoid oversulphonation due to fluctuations; (20%
more than nominal).
- Open the relevant valves for LAE feeding on storage tank and close
the relevant valves for the LAB feeding, taking care to avoid any lack
or fluctuation on the raw material feed.

8 Take under control the colour of product outflowing the bottom of 16R1;
when become dark-red, send the product to the OFF-specs cubitainer

9 Within few minutes the product colour will become clear again (indicating
that all the LABS went off and only LAE is flowing). Change again the valves
position sending the product directly to neutralization unit.

10 Take care to adjust the operating parameters on neutralization unit

according to the new production.

11 Enable the EMERGENCY on 16R1.

NOTE 1
The above procedure was applied to a specific case of production but it is
similarly carried out for any other production quality and production, by varying
the process parameters, according to the stoichiometric ratios.
Change over between two alcohols is easier, because they can be mixed
without affecting their quality.

SHUT-DOWN CHANGE OVER

Procedure

1. Switch into manual PIC 16.1 (if in operation) and DISABLE THE
EMERGENCY SEQUENCE
2. Change the raw material feed to the reactor. Proceed as follows:
- Open the relevant valves for LAB feeding on storage tank and close
the relevant valves for the LAE feeding, taking care to avoid any lack
or fluctuation on the raw material feed
- Divert the acid flow to the off-spec cibitainer and close the feeding
valve to neutralization unit
- Shut down the neutralization unit and the deaeration section (if in
operation)
 1E55-40-600 OPERATION HANDBOOK 109

3. Adjust the SO3 gas flow at the new operating set point.
4. Decrease the dilution air down to the new operating set point; variation
on the SO3 and air gas flows must be carry out with care, avoiding big
variations on the pressure of the circuit.
5. Set the sulfur flow rate per LAB process.
6. During this period (around 30 minutes), the conversion degree could
decrease due to catalysis temperatures variations; that means it is
advisable to take under deep control the acid value of product outflowing
16R1, untill all parameters are stable.
7. Adjust gradually the raw material flowrate, in order to maintain the correct
acid value. Keep under control the density variations on DI16.4..

CAPACITY INCREASE

Increase of sulfur dosing without changing the raw material.

- Increase the raw material feed (FIC16:3).

- Increase the gas flowrates (FIC16.2 and FIC16.1). Take under control
the pressure variation on PIC16.1 and adjust it accordingly
- Increase the sulfur flowrate (FIC25.1).

Moreover, increase the caustic soda dosing (adjust accordingly the piston
stroke on head "C" of 17P1) .
Increase the process water dosing (adjust accordingly the piston stroke on head
"A" and "B" of 17P1).

CAPACITY DECREASE

Decrease of sulfur dosing without changing the raw material.

- Decrease the sulfur flowrate (FIC25.1).

- Decrease the gas flowrates (FIC16.2 and FIC16.1). Take under control
the pressure variation on PIC16.1 and adjust it accordingly.
- Decrease the raw material feed (FIC16:3).

Moreover, decrease the process water dosing (adjust accordingly the piston
stroke on head "A" and "B" of 17P1).
Decrease the caustic soda dosing (adjust accordingly the piston stroke on head
"C" of 17P1).

NOTE: all the variations must be done in short time, in order to reduce at
minimum the OFF-specs production (Free oil content).
 1E55-40-600 OPERATION HANDBOOK 110

10. Emergency shut down

10.1 Introduction
In this paragraph, the most important emergency procedures which, according to Ballestra
experience, may occur during sulphonation plant running are described.
The Ballestra plant can easily be stopped and restarted in a short time, even without
warning. For this reason, emergency situations cannot be dangerous to either personnel
nor the plant.
The only precaution to be assumed is to avoid the charring of the film reactor's heads, due
to oversulphonation of the organic material inside the heads.
To prevent this possibility, a proper fully automatic emergency system is foreseen on the
film reactor. Make reference to the URS (see ANNEX ) for detailed explanation.

10.2 Raw material feeding failure to 16R1

The emergency procedure is enabled from low organic material flowrate, detected by the
flow element FIC 16.3 and proceeds as follows (see Reactor emergency sequence, URS) :
valve KV16.1 close;
FV 16.3 100% open
11K1 and 25P1/2 stop;
pumps 16P2 , 16P3 , 16P4 , 17P1 , 17P2 , 07P1 stop;
raw material feed pump stop;
KV 16.4 open
At the end the plant is under safety conditions; detect the causes of the shut down and
remove, before re-start.

10.3 Air blower 11K1 troubles

The air blower 11K1 shut down is a critical situation for the safety operation of the plant;
therefore the following emergency interlocks were foreseen:
- stop sulphur pumps 25P1/25P2, so that putting under safety conditions the plant.
- stop the chilling group 11RG1, so that avoiding that moisture eventually present inside
freezes on the coils due to the glycol solution circulating at 0°C .

The plant is under safety conditions; the operator will provide to stop the other sections of
the plant.
Sulphonation plant may also be re-started in a short time, taking into account that pre-
heating is not needed if the temperature at first catalyst layer inlet of the conversion tower
12C1 is higher than 350°C.

10.4 Power failure

As already explained under paragraph 8.2, in case of black-out, all the equipment of the
plant stop immediately; the sequence will be achieved by low flow signal from FIC 16.3.
 1E55-40-600 OPERATION HANDBOOK 111

11. Troubleshooting

As explained under chapter 8, the film sulphonation plant is provided with an emergency
system to obviate the trouble due to failure of electric power and/or raw material.
More detailed informations about emergency sequences and all other interlocks to service
of the plant, are reported in the manual " USER'S REQUIREMENTS SPECIFICATION"
enclosed as Annex. However, during the plant running the operator may have to face other
several troubles, that are mainly the following:
 1E55-40-600 OPERATION HANDBOOK 112

TROUBLE PROBABLE ACTION

CAUSE
High pressure at blower 1. Packing flooding on  Check the pressure
11K1 14C1. drops on the plant

2. Sulfur furnace refractory

balls clogging.

3. Catalyst beds high

pressure drop.

4. SO3 cooler fouling.

Low pressure at 1. Air filter 11F1 Check the pressure

compressor 11K1 clogging between blower and air
filter; if needed replace air
filter

High/low temperature of 1. Thermometers out of  Check the

glycol entering into the calibration thermometers
chiller 11RG1
2. Temperature controller  Set the control loop;
is not properly set
 Replace or repair the
3. Temperature controller instrument defective.
out of order
 Verify that the suction
4. Circulating pump flow valve is open and no
is not sufficient clogging are along
delivery lines

No water is discharged 1. Temperature is too  Adjust the set

from cooling batteries low, thus causing temperature
container 11V2 (pipe condensate frozen. accordingly
SD11106)
2. Valves and/or  Check valves and
electrovalves are electrovalves operate
closed or do not properly.
operate properly.
 1E55-40-600 OPERATION HANDBOOK 113

TROUBLE PROBABLE ACTION

CAUSE
Low temperature of air 1. Steam low pressure  Check the pressure
coming from 11E1battery indications and
(seeTI11.7) , when 2. By-passes of steam operation of the
regeneration is carried out traps are open pressure reducing
by means of steam valve if any.
3. Air valve open too much
(pipe AT11017)  Close by pass valves

 Reduce operating on
related valve

High regeneration 4. Defect of atmospheric  Open the related valve

temperature air (see pipe AT11017)

5. Hot air flow from  Dilute the air flow to

catalisys too high (if silica gel beds by
recover is operating means of atmospheric
via pipe AH12026) air (see pipe AT11017)

Water hammering in 11V2 1. Water is not  Check the non return

discharged from the valve on water
cooling batteries discharge pipe
WR11106.

High temperature of 1. High pressure of  Operate on the

sulphur steam pressure reducing valve
PCV25.1.

Sulfur pump 25P1 or 25P2 1. Level inside vessel  Check and operate
does not give any flow 25V1 is too low. accordingly

2. Valve on suction is  Open the suction valve

closed.
 Open steam on the
3. Steam on suction suitable valve.
pipe is closed.
 Clean the filter.
4. Sulphur filter clogged.

Sulfur pump does not give 1. Ball valves are dirty.  Start stand-by pump
any precise flow and clean the piston
head.
 1E55-40-600 OPERATION HANDBOOK 114

TROUBLE PROBABLE ACTION

CAUSE
A lot of quantity of 1. Furnace is still cold.  Wait for some hours
dripping sulfur on the before taking actions
bottom of furnace 12H1. 2. Process air velocity is
low.  Increase the plant
capacity or decrease
the SO2 concentration.

High temperature at outlet 1. High SO2 concentration  Check the ratio of air
of sulfur furnace 12H1 and sulfur

Low temperature on 1 Low SO2 concentration.  Reduce the air stream

furnace outlet to furnace.
2 Lack of sulfur.
 Check sulfur pump.

Low conversion of SO2 to 1. Wrong temperature at  Check if the

SO3 inlet of catalysis temperatures are close
stages to optimal

2. Progressive loss of  Open the tower,

efficiency of the ventilate the catalyst
catalyst and add new one.

Formation of oleum 1. Moisture in the  Check the correct

conversion gas unit operation of the chilling
group 11RG1 and the
efficiency of the drying
tower, by measuring the
2. Leakage of steam in air dew-point after silica
the sulfur lines gel bed. Check MIT11.1
and make new
calibration
3. Water leakages in the
 Verify if there is any
cooling battery inside
leak of steam in the
11V2.
sulphur pumping
section

 Check the cooling

battery
 1E55-40-600 OPERATION HANDBOOK 115

TROUBLE PROBABLE ACTION

CAUSE
High pressure alarm 1. Filter 16F3 is obstructed  Remove carefully the
downstream 12E6 filtering element from filter
detected from pressure 16F3 (oleum mists
alarm PSH12.1. separator). Replace it.

High pressure in the 1. Package of pall rings on  Increase the flow of dilution
exhaust gas line tower 14C1 is partially water in tower 14C1 so
(pressure indication on obstructed by sodium that diluting the recycle
PI14.1) sulphite crystal. (check solution to approx. 10% as
load loss in the tower). sodium sulphite content
(suitable operation conc.)

Decrease of pressure 1. Leakage in the SO3  Verify the leakage and if

on the SO3 gas line to circuit and/or in the possible, repair it. In case it
the film reactor dilution air circuit is an air leak, increase the
flow if possible, to have the
2. Defect on the by-pass same quantity to the
valve of blower reactor.

 Close the by pass valve.

High pressure on the 1. Combustion air quantity  Clean and calibrate the
SO3 gas line to the film is too high (FE16.2 FE16.2 (keeping into
reactor. clogged or FV16.2 fault). manual the loop FIC16.2.
Check the air/SO3 ratio;
2. Defect on the valve for adjust the valve manually.
gas inlet to the reactor
KV 16.5  Check the pressure set
point on PIC16.1;
3. Clogging of the SO3
filter 16F3 (check the  Check the instrument air
inlet and outlet pressure and, if
pressure). decreased, increase it; if
there is any air leak seal
them.

 Stop the sulphonation

plant. Remove carefully
filtering element and
replace it.
 1E55-40-600 OPERATION HANDBOOK 116

TROUBLE PROBABLE ACTION

CAUSE
Quick decrease or increase of 1. Defect on the cooling  Check and
the gas temperature. SO3 section valves. adjust

Note: the SO3 gas temperature has not to drop or rise too
much, but it has to remain within the running limits
(48°C- 52°C - detected from TI16.1).

High gas emissions on 1. Recycle solution in  Increase the quantity of

chimney of scrubber 14C1. column 14C1 is acid. caustic soda in the
recycle solution to
2. Flow rate of pump 14P1 maintain 10-12 as pH .
is insufficient or the
pump does not work.  Check the pump
impeller and replace it
3. Poor converter eventually. Besides,
operation. check that no crystal
forms in the pump
section.

 Check temperatures in
the catalysys tower to
get optimum conversion.

The raw material 1. Failure of heating  Check if tracing lines

tends to solidify due water to the lines on valves are closed.
to low temperature day tank
 Verify the operation of
the hot water production
unit.

Note: If the raw material entering the reactor head has a

temperature approaching the freezing point, the reactor
could get out of balance, causing over sulphonation in
some of the tubes, due to the closing of the slots
forming the film; change the delivery of the feeding
pump, thus unbalancing the ratio of gas/raw material
 1E55-40-600 OPERATION HANDBOOK 117

TROUBLE PROBABLE ACTION

CAUSE
High production of oleum 1. High presence of  Check the dew point of
moisture in the the process air and
process air silica gel operation;
verify possible water
leaks in the air cooling
battery (11V2)

The temperature of the 1. Failure of cooling  Check the water flow

acid coming out of the H2O to the reactor indication on FI16.5 and
reactor increases quickly. temperature indication
on TI16.5 – TI16.6 -
TI16.4

Note: If the failure is temporary, the acid will become dark,

but it will be possible to go on running if the cooling
water circulation is restored in few time; otherwise,
stop the plant.

2. Excess of reaction.  Check the sulphonation

degree and parameters of
operation.
3. Raw material too hot.  Check the temperature of
raw material

 Check the good operation

4. Temperature control of TIC 16.7/TV 16.7. If it
system for cooling
cannot be repaired verify
water is out-of the water temperature
calibration (TIC16.7) through regulation of the
by-pass valve of TV 16.7.

The temperature of 1. Shortage of cooling  Verify the discharge

cooling water outflowing water temperature valves from reactor;
the reactor stages increase). check the pressure
increases or decreases indicator PI16.9 on the
quickly 2. Defect in the recycle pump 16P1.
thermostating system
(increase of  See the control system
temperature). TIC16.7/TV16.7 .

3. Direct steam enters into  Check leaks of steam

the line (increase of injection valve on cooling
temperature). circuit (pipe VB16110).
 1E55-40-600 OPERATION HANDBOOK 118

TROUBLE PROBABLE ACTION

CAUSE
The acid product results 1. Gas raw-material  Verify: the gas raw
dark and ratio is out of material flow meters and
oversulphonated balance. running parameters to
restore the right
stoichiometric ratio.
2. Failure of cooling H2O  See previous point
to the reactor.
 Increase the flow of raw
3. The heads forming material through the raw
the film are out of material feeding pump
balance (due to for some seconds,
possible fouling, check if the product
foreign matters) coming out brightens
and restore the
stoichiometric flow. If the
washing was sufficient,
the heads are clean and
the operation can go on;
otherwise, it will be
necessary to stop and
clean the reactor.

The produced acid Gas / raw material  See previous point..

outflowing is not fully ratio is out of
sulphonated. balance.

The produced acid results 1. Presence of H2O in  Check the analysis of

dark and increase the the raw material, H2SO4 present in the
quantity of exhaust gas causing high H2SO4 acid and the H2O
considerably. in the product. content in the raw
material. If the value of
2. Presence of water H2SO4 is high, replace
from catalysys. the raw material.

 Check H2SO4 analysys;

check the drying section
efficiency.
1E55-40-600 OPERATION HANDBOOK 119

12. Annexes
ANNEX 1 : USER’S REQUIREMENT SPECIFICATION, spec 1E55-40-280

ANNEX 2 :HEAT & MATERIAL BALANCE, spec 1E55-40-277

ANNEX 3 :AIR DRYING UNIT (item 11C1 ) Ballestra Standard Procedures.

Spec : SB-PRO-C0002 – AIR DRYING UNIT.

ANNEX 4 :SULPHUR FURNACE CURING (item 12H1 ) Ballestra Standard

Procedures. Spec.: SB-PRO-H0001 - SULPHUR FURNACE

ANNEX 5 : SO2 / SO3 CONVERTER COLUMN (item 12C1) Ballestra Standard

Procedures. Spec.: SB-PRO-C0001 - SO2 / SO3 CONVERSION
COLUMN.

ANNEX 6 : SO3 COOLERS (item 12E5/6) Ballestra Standard Procedures.

Spec.: SB-PRO-E0001 – CLEANING PROCEDURE FOR SO3
COOLERS.

ANNEX 7 : SO3 FILTER (item 16F3) Standard Procedures. Spec: SB-PRO-

F0003 - SO3 BRINK FILTER.

ANNEX 8 : FILM REACTOR (item 16R1) Ballestra Standard Procedures.

Spec.: SB-PRO-R0001 - FILM REACTOR PRE-
COMM./COMM.&MAINTENANCE.

ANNEX 9 : ESP (item 14F1 ) Ballestra Standard Procedures. Spec.: SB-

PRO-F0001 ESP ELECTROSTATIC PRECIPITATOR - ITEM
14.F.1 - MECHANICAL HANDBOOK.

ANNEX 10 : MOLTEN SULPHUR TANK (item 25V1) Ballestra Standard

Procedures Spec.: SB-PRO-V001 - SULPHUR MELTING TANK
- ITEM 25.V.1 - OPERATION & MAINTENANCE HANDBOOK.

ANNEX 11 : NEUTREX MIXER 17MX1 AND DILUTION MIXER 22MX1

MECHANICAL SEAL PRESSURE VESSEL Ballestra Standard
Procedures. Spec.: SB-PRO-MX001 - START-UP PROCEDURE
FOR OPPOSED DOUBLE MECHANICAL SEAL STIRRERS
(BALANCED TYPE).