Chemical Engineering and Processing 43 (2004) 647653

Selection of inherently safer process routes: a case study

Chidambaram Palaniappan, Rajagopalan Srinivasan , Reginald Tan
Laboratory for Intelligent Applications in Chemical Engineering, Department of Chemical and Environmental Engineering,
National University of Singapore, 10 Kent Ridge Crescent, Singapore 119260, Singapore
Received 17 July 2002; received in revised form 12 December 2002; accepted 30 December 2002

Abstract
Increased public concern about safety issues and stringent environmental standards has led plant designers to consider inherently safer
design. The term inherently safer implies that the process is safe by its very nature and not externally constrained to be safe by the use of
add-on systems and devices. Such opportunities for developing inherently safer process are highest in the early stages of design. Constraints
such as time, lack of knowledge and inadequate inherent safety analysis tools are often cited as obstacles to development and implementation
of inherently safer design. In this paper, we describe an inherent safety analysis methodology that can be applied in the early stages of process
development. The methodology is based on an inherent safety index for comparing process routes and heuristics for identifying hazards and
generating alternative designs. This methodology has been implemented as one module in iSafe, an intelligent system that automates inherent
safety analysis. One key benefit of iSafe is substantial reduction in the time and effort required to perform safety analysis. Automation of the
inherent safety analysis also makes it more thorough and detailed, minimizes or eliminates human errors, facilitates documentation and makes
the study results available online for detailed safety analysis and review in the later stages of process design. The details of inherent safety
analysis at the route selection stage are discussed in this paper and illustrated by comparing competing processes for acetic acid manufacture.
2003 Elsevier B.V. All rights reserved.
Keywords: Inherent safety; Process design; Route selection; Acetic acid process

1. Introduction
In recent years, the risks posed by chemical industries
to life, property and environment has significantly increased due to many reasons: increased population density
near industrial complexes, size of operation, complexity,
and use of extreme operating conditions. This has led
to the development and use of better hazard identification and analysis techniques like FMEA, QRA, HAZOP,
etc. which try to reduce the frequency and consequences
of accidents. Such safety analyses at later stages complicate the design and prompt additional costs. Estimates
show that in the oil and chemical industries, 1530%
of capital cost is now spent on such safety and pollution prevention measures [1]. This has challenged chemical industries to develop processes that are inherently
safer, environmentally friendlier, simpler, and more cost
effective.

Corresponding author. Tel.: +65-687-480-41; fax: +65-677-919-36.

E-mail address: chergs@nus.edu.sg (R. Srinivasan).

0255-2701/$ see front matter 2003 Elsevier B.V. All rights reserved.
doi:10.1016/j.cep.2002.12.001

An inherently safer process avoids or reduces hazards

instead of controlling them. It relies on naturally occurring
phenomena and robust design and eliminates or greatly
reduces the need for instrumentation or administrative
controls, thereby reducing the costs related to safety and
environment. This is normally accomplished by application
of inherent safety principles throughout the design process,
from conception until completion. Examples of the principles are intensification, substitution, attenuation, limitation
of effects, simplification, etc. These principles help avoid or
reduce hazards by using safer materials and operating conditions, minimizing inventory, and by designing a simpler and
friendlier plant. Opportunities for identification and development of inherently safer process alternatives for solvents,
reaction paths, catalyst, etc. are high during the early design
stages. Decisions made during early design stages concerning the choice of a synthesis route for a product, location for
manufacture, and throughput are crucial and fix 80% of capital cost [2]. The benefits realized by industrial application
of inherent safety concepts have been discussed by several
authors [35] and include improved public image, reduced
life-cycle cost, improved productivity, increased reliability,

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reduced company liabilities, and improved safety and environmental performance. Despite the obvious importance of
inherently safer design, there has only been limited work on
development of support tools for inherent safety analysis.
We have developed an intelligent design support system,
called iSafe, for performing inherent safety analysis during
early stages of design. iSafe identifies hazardous issues and
proposes inherently safer alternatives to eliminate or reduce them. While iSafe can be used throughout the design
life-cycle, the focus in this paper is on the route selection
stage, specifically, ranking competing routes from the safety
perspective. The organization of this paper is as follows.
In Section 2, an overview of process design and inherent
safety is presented. In Section 3, we illustrate the index
and heuristics based approaches implemented in iSafe for
evaluating processes using the example of competing acetic
acid processes. Conclusions from this study are presented
in Section 4.

2. Process design and inherent safety

A process goes through various stages of evolution,
including research, process development, design, construction, operation, maintenance, modifications, and finally,
decommissioning. An inherently safer process design and
development methodology involves iterative application of
chemical engineering and inherent safety principles at each
decision point along the process life-cycle. The key decision points include: (1) product specification; (2) synthesis
route selection; (3) flowsheet development; (4) conceptual
design; (5) detailed engineering; and (6) construction and
commissioning. Traditional process design addresses specific issues one at a time and revisions are made to the
design, as constraints and opportunities are recognized.
Cost of the product and raw material and process yield are
some of the metrics used at early stages to screen routes for
a specific product. Safety usually plays a passive role and
acts as a verification criterion for the final design. The shift
from traditional sequential design to concurrent design has
contributed to the adoption of inherent safety measures for
hazard elimination or reduction instead of risk reduction
through addition of layers of protection.
Screening of process routes is critical for inherently safer
design. In order to rank process routes at early stages,
Edwards and Lawrence [6] developed an index, called prototype index for inherent safety (PIIS), based on parameters
that influence inherent safety of a process route. A low
value of index means high degree of inherent safety. One
key drawback of PIIS is that it concentrates on reactions
and does not consider other process aspects. Heikkila [7]
overcame this by considering a wider range of factors affecting the inherent safety of the process in the inherent
safety index (ISI). ISI accounts for process safety structure,
side reactions, corrosiveness, chemical interaction, type of
equipment, and inventory based on annual throughput in-

stead of yield. It is thus applicable to both route selection

and flowsheet stages. An index serves as a yardstick that
reflects change in magnitude and direction of individual
hazards due to changes made to the process. It also serves
as a guide for the design team to set priorities for further
design work. The index calculation is not sufficient in itself
to make a decision on the choice of a process route. Detailed
inherent safety analysis of each process routes is necessary
to identify hazards and alternatives to rectify them.
A review of the status of inherently safer process design
in the UK conducted by Health and Safety Executive resulted in the European Community co-funded project, called
INSIDE, to develop tools and methodologies for systematic
application of inherent safety [8]. The INSIDE project resulted in the development of a paper-based tool-kit, called
INSET, which facilitates the application of inherent safety
principles along the process life-cycle. Despite the growing
interest and obvious importance of inherently safer design,
its adoption into practice has been slow. The main barriers
for adoption of inherently safer approaches are time and
cost pressures on project that do not allow for systematic
study of alternatives during the early stages, conservatism
in design and management, lack of awareness and lack of
support tools [810]. Rushton et al. [11] emphasized the
need for a computer aid that will perform comprehensive
inherent safety analysis at each key decision point in the
process life. The key benefits of automation are substantial
reduction in time and effort, enhanced decision-making,
improved documentation, and better understanding of the
process. Towards this, we have developed an intelligent
design support tool, called iSafe, that automates inherent
safety analysis during early stages of design [12,13]. iSafe
can rank competing process routes using an inherent safety
index and also assist the designer identify safety issues and
design alternatives during the different stages of the design
life-cycle. The methodology implemented in iSafe for analyzing process routes is explained in the next section and
illustrated using competing acetic acid processes.

3. Inherent safety analysis of process routes

using i Safe
Process route selection is the heart of the design process.
During this stage, the process configurationreactor, separation units, and the need for recycleand thus the raw materials, byproducts, intermediates, catalysts and the reaction
conditions are determined. The inherent process hazards are
thus largely fixed during this stage. iSafe identifies the hazards that are associated with the reactions and the chemicals
involved in the process route and ranks the available process
routes for the product chosen in the product specification
stage. Information used for analysis are reaction conditions,
materials involved, heat of reaction, catalysts, phase of reaction, unit process involved, and process yield. Examples
of unit processes include chlorination, nitration, oxidation,

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649

Table 1
Details of acetic acid process routes [1418]
Process name

Reactions involved

Reaction conditions
Temperature
( C)

Halcon vapor phase

oxidation
Ethylene oxidation
Butane oxidation
Huels butene oxidation

Acetaldehyde oxidation
Ethane oxidation
Ethanol oxidation
Low-pressure
carbonylation
High-pressure
carbonylation
Methane oxidation

Ethylene + oxygen
acetic acid
Ethylene + oxygen
acetic acid
Butane + oxygen
acetic acid + water
Butene + oxygen
acetic acid + formic
acid
Acetaldehyde + oxygen
acetic acid
Ethane + oxygen
acetic acid + water
Ethanol + oxygen
acetic acid + water
Methanol + carbon
monoxide acetic acid
Methanol + carbon
monoxide acetic acid
Methane + oxygen
methanol + carbon
monoxide + water
Methanol + carbon
monoxide acetic acid

215250
150
150200

Pressure
(atm)
1020
4.5
56

Hr
(kJ/g)

Catalyst

Reaction
phase

Process
yield

PdCl2 and
vanadium oxide
Pd and H3 PO4

Vapor

60

6.374

Vapor

80

6.374

Cobalt acetate

Liquid

75

8.185

180240

230

Titaniumvanadium
oxide

Vapor

46

4.4

6080

310

Manganese acetate

Liquid

95

4.528

150450

1530

NAa

Gas

25

9.809

60115

14

Cobalt acetate

Liquid

90

7.593

150200

415

Rhodium iodide

Liquid

99

1.532

Cobalt iodide

Liquid

99

1.532

NA

Gas

NA

12.296

250

700

350500

60100

150250

11.5

Rhodium iodide

1.532

Not available.

carbonylation, polymerization, etc. Process routes available

for manufacture of a chemical can be ranked using inherent
safety indices. iSafes route index is based on the scoring
pattern used in ISI [7] which enables uniformity in index
values across design stages.
3.1. Index calculation for acetic acid process routes
The application of iSafe is illustrated through the comparison of ten different acetic acid process routes [1418]
in this section. The reactions involved in each process route
along with the information used for the inherent safety analysis are shown in Table 1. The index for individual route
options was calculated and safety issues associated with
the processes and inherently safer alternatives to reduce
hazards were identified using iSafe. The index calculation
methodology is illustrated for the low-pressure carbonylation process in Tables 2 and 3. The overall safety index
(OSI) accounts for the hazards due to the chemicals in a
process route and reaction conditions. The OSI does not
take into account safety issues related to factors such as: (1)
phase of reaction; (2) use of catalyst and solvent; (3) phase
generation; (4) byproduct formation; (5) auto-ignition; (6)
decomposition; and (7) type of unit process involved in the
chemistry. The individual chemical index (ICI) characterizes each chemical involved in a route whereas the individual reaction index (IRI) characterizes reaction. Scores for
calculating sub-indices involved in calculation of ICI and

IRI are taken from Heikkilas ISI [7] except for the process
yield index, which is from Edwards and Lawrences PIIS
[6]. During early design stages, information of inventory
is usually lacking and reaction yield can be used as a measure of inventory since higher yield results in reduction
in the size of reactors and recycles. Scores for flammability index and process yield index are shown in Tables 4
and 5, respectively. The indices calculated by iSafe for each
route is shown in Table 6. The overall reaction index (ORI)
characterizes the hazardous conditions in the process route.
The ORI for a process route is high when it involves large
number of main reactions. Therefore, a route with a smaller
number of reactors (corresponding to a few main reactions)
is preferred over one with many. This will help in focusing
on the reduction of inventory of hazardous chemicals and
elimination of hazardous reactions. The hazardous chemical index (HCI) and the hazardous reaction index (HRI) are
indicators of the most hazardous chemical and reaction in
the process route. The value of HCI and HRI will be same
as ORI and OCI if there is only one reaction in the route.
The method of calculating OSI does not differentiate between routes based on the number of chemicals or reactions
and their hazardous properties. We overcome this limitation by introducing three additional supplementary indices
worst chemical index (WCI), worst reaction index (WRI),
and total chemical index (TCI). The WCI is the summation
of maximum values of the flammability, toxicity, reactivity,
and explosiveness indices of all the materials involved in a

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Table 2
Illustration of index calculation for low pressure carbonylation route
Component of inherent
safety index [12]

Notation

Equation (see [12])

Index calculation

Index value

Individual chemical index

ICI

Nr + Nf + Nt + Ne

10

Individual reaction index

Hazardous chemical index
Hazardous reaction index
Overall chemical index
Overall reaction index
Overall safety index
Worst chemical index

IRI
HCI
HRI
OCI
ORI
OSI
WCI

Worst reaction index

WRI

Total chemical index

TCI

R t + Rp + Ry + Rh
max(ICI)
max(IRI)
max(ICI)



IRI
(OCI + ORI)
max(Nr ) + max(Nf )
+ max(Nt ) + max(Ne )
max(Rt ) + max(Rp )
+ max(Ry ) + max(Rh )


ICI

0 +4 +3 +3
(for carbon monoxide, see Table 3)
2 +1 +1 +3
max(8, 7, 10) (see Table 3)
7
10
7
10 + 7
1 + 4 + 4 + 3 (see Table 3)

7
10
7
10
7
17
12

2 +1 +1 +3

8 + 7 + 10 (see Table 3)

25

Nr : NFPA reactivity rating; Nf : flammability index; Nt : toxicity index; Ne : explosiveness index, Rt : temperature sub-index; Rp : pressure sub-index; Ry :
yield sub-index; Rh : heat of reaction sub-index.
Table 3
Subindex for chemicals in low pressure carbonylation route
Chemical

Reactivity
index (Nr )

Flammability
index (Nf )

Toxicity
index (Nt )

Explosiveness
index (Ne )

Individual chemical
index (ICI)

Acetic acid
Carbon monoxide
Methanol
Max(index)

1
0
0
1

2
4
3
4

4
3
2
4

1
3
2
3

8
10
7

reaction step. Similarly, the WRI is the sum of the maximum

of the individual indices of temperature, pressure, yield, and
heat of reaction of all the reactions involved in the process.
The TCI is a measure of the number of hazardous chemicals
involved in the route. That is, a route with just one highly
toxic chemical is safer compared to another route with several toxic chemicals. WCI and the TCI are calculated for all
the chemicals in the process route. The OSI along with the
three supplementary indices are used to rank process routes
as follows. Routes are first ordered according to OSI. For
cases where two competing routes have similar OSI, the supplementary indices are then compared. While the relative
weightage of the three supplementary indices is subjective,
we have weighted TCI, WRI, and WCI in that order.
Based on the index calculation, it can be concluded that
ethanol oxidation is the inherently safer route and methane
oxidation the most hazardous one. The methane oxidation
Table 4
Heuristics for flammable nature and index calculation [7]
Condition
>55 C

Flash point
Flash point 55 C
Flash point <21 C
Flash point >0 C, boiling
point 35 C
Flash point (not defined)

Flammable nature

Score

Combustible
Flammable liquid
Easily flammable
Very flammable

1
2
3
4

Non-flammable

route is a two-step process while the others are single-step

processes. By comparing the OSI values, the methane oxidation process can be concluded to be the most hazardous
one. The OSI values for the low-pressure carbonylation,
Acetaldehyde oxidation, Halcon vapor phase oxidation,
high-pressure carbonylation and butane oxidation are close
to each other. The OSI for the low-pressure carbonylation
process is lower than that of the Halcon vapor phase oxidation process while the low-pressure carbonylation process
TCI is higher. The higher TCI for the low-pressure carbonylation process is due to the use of a large number
of hazardous chemicals. Since the WCI of these two processes are the same and information on inventory of each
Table 5
Heuristics for process yield index calculation [6]
Process yield (%)

Score

100
9099
8089
7079
6069
5059
4049
3039
2029
1019
010

0
1
2
3
4
5
6
7
8
9
10

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651

Table 6
Summary of index calculations for acetic acid processes
Process

Heat of
reaction
index

Pressure
index

Process
yield
index

Temperature
index

Ethanol oxidation
Ethylene oxidation
Low-pressure
carbonylation
Acetaldehyde oxidation
Halcon vapor phase
oxidation
Butane oxidation
High-pressure
carbonylation
Huels butene oxidation
Ethane oxidation

4
4
3

0
0
1

1
2
1

1
1
2

4
4

1
1

1
4

4
3

3
4

4
4
4
3

Methane oxidation
a

Overall
reaction
index

Overall
chemical
index

Overall
safety
index

Total
chemical
index

Worst
reaction
index

Worst
chemical
index

6
7
7

8
8
10

14
15
17

14
16
25

6
7
7

9
12
12

0
2

6
11

12
8

18
19

20
16

6
11

13
12

3
1

2
2

12
10

8
10

20
20

15
25

12
10

10
12

1
1

6
8

2
2

13
15

8
8

21
23

21
13

13
15

11
10

2
0

NAa
NA

3
2

9
5

7
10

31

32

12

Not available.

hazardous chemical in the process is not available during this stage, their WRI are compared which reveals that
the low-pressure carbonylation process is inherently safer.
Similarly, processes can be ranked based on worst possible combination of reaction conditions using WRI. Since
the low-pressure carbonylation process involves one main
reaction, values of IRI, HRI, and WRI are equal.
3.2. Hazard identification and alternative generation
for acetic acid processes
While the inherent safety index provides a quantitative
perspective, a qualitative perspective can reveal specific
safety issues associated with a route, which can then be
eliminated by using alternate safer design options. iSafe can
automatically identify safety issues and suggest alternative
designs. These are identified by iSafe using heuristics based
on inherent safety principles. A part of the heuristics used
during the route selection stage is shown in Table 7. The
inherent hazards related to materials are identified based
on their physical, toxicological, chemical, and reactive
properties. A material is concluded to be hazardous if it
is flammable, carcinogenic, teratogenic, mutagenic, water
reactive, unstable, pyrophoric, corrosive, toxic, or explosive. For example, toxic carbon monoxide involved in the
low-pressure carbonylation route and flammable ethylene
involved in the Halcon vapor phase oxidation process are
concluded as hazardous. Alternatives such as use safer
material and modify hazardous material into less hazardous form are suggested for a hazardous product to
minimize or eliminate hazards. The phase of a reaction
influences the dispersion characteristics in case of leak in
the reactor system. For liquid phase reactions like lowand high-pressure carbonylation processes, the use of vapor
phase can be recommended. This is because the mass of
material released for the same volume is smaller compared

to liquid phase under the same conditions. Waste products

from reactions need to be reduced in order to reduce wastage
of raw materials and decrease the reactor size required for
the same throughput. If a material produced in the reaction
is a byproduct then improve process yield is proposed as
an alternative. Improvement of yield is thus proposed for
the Huels butene oxidation process. The use of catalysts
may increase yield and allow reactions to be carried out at
safer conditions. Therefore, if a process is non-catalytic and
yield is low then use of a catalytic process is proposed. In
the case of Huels butene oxidation process with low yield,
change of catalyst to improve yield is suggested. Catalysts
can be a hazard by themselves. For example, commonly
used heavy metal catalysts are potentially poisonous. The
hazards related to catalysts and solvents used in the reaction are evaluated similar to other materials. Heuristics are
also used to identify hazards associated with common unit
processes. Possibility of explosion in the ethylene oxidation process is identified due to handling of oxygen and
flammable materials and possibility of thermal runaway
due to exothermic reaction in the case of high-pressure
carbonylation are highlighted.
Additional information about the process hazards generated during the index calculation can be supplemented
with additional heuristics to diagnose hazards and suggest
alternatives. The premise underlying the index-based issue
identification is that any sub-index value greater than one is
considered hazardous and an alternative has to be explored.
For example, if the process yield index is greater than one,
then low process yield is highlighted as an issue, and improve process yield is suggested as an alternative. Issues
such as the use of extreme operating conditions and release of large amount of heat are identified. Inherently safer
alternatives to minimize them such as look for safer process chemistry, use safer operating conditions, and use
high yield process can then be proposed. High-pressure

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Table 7
Extract of heuristics for hazards and inherently safer alternatives identification in iSafe
Applicable item

Condition

Safety issues

Alternative

Raw material/intermediate/
catalyst/solvent

Hazardous material
Flammable material

Use of hazardous material in

reaction
Possibility of fire and explosion

Corrosive material

Corrosion of equipment

Look for a process chemistry

that uses safer material
Replace material with a safer
material
Change material with a safer
material by either changing or
masking material structure,
form, phase or by dilution

Toxic/mutagenic/carcinogenic/
teratogenic material
Reactive/polymerisable/
pyrophoric/peroxide
forming/water
reactive/thermally unstable

Possibility of toxic vapor cloud

formation
Possibility of unintended
reactions

Reduce the reactivity of material

by using stabilizers or inhibitors

Solvent

Hazardous solvent

Use of hazardous solvent

Use of solvent-less process

Reaction

Liquid phase catalyst

Increases in exposure potential

Temperature index >1, or

pressure index >1
Heat of reaction index >1

Use of extreme operating

conditions
Release of large amount of
energy
Process yield is low

Use solid or polymer supported

catalyst
Look for process chemistry with
safer operating conditions
Look for process chemistry that
releases less energy
Look for a higher yield process

Process yield index >0, and

catalytic reaction
Process yield index >0, and
non-catalytic reaction

Use
will
Use
will

of alternate catalyst that

improve yield
of catalytic process that
improve yield

Table 8
Sample results from iSafes analysis of Halcon vapor phase oxidation process
S. no.

Issue

Alternative

Unit process oxidation is highly exothermic and there is likelihood

of fire and explosion hazards

Look for a safer process chemistry

Use of hazardous material ethylene in the reaction in Halcon vapor

phase oxidation process

Replace the hazardous raw material ethylene with a safer material

by either changing or masking material structure
Replace the explosive raw material ethylene with a safer material
or material with higher lower explosive limit and narrower range
of explosive limits
Replace the flammable raw material ethylene with a safer material
Look for a process chemistry that uses safer materials
Replace the reactive raw material ethylene with a safer material
Reduce the possible unintended reactions of reactive ethylene by
using stabilizers or inhibitors

Process yield is low

Use catalytic process that will improve yield

Look for a process chemistry with higher yield

Release of large amount of thermal energy in Halcon vapor phase

oxidation process and possibility of pressure increase and loss of
temperatures exists

Look for safer process chemistry that releases less energy

Consider use of biocatalyst/enzyme catalyst or phase transfer

catalyst which involves milder reaction conditions
Use alternate catalyst that will alter the reaction conditions in
without affecting selectivity
5

Handling of chemicals at extreme operating conditions in Halcon

vapor phase oxidation process

Look for safer process chemistry that releases less energy

Consider use of biocatalyst/enzyme catalyst or phase transfer
catalyst which involves milder reaction conditions
Use alternate catalyst that will alter the reaction conditions in
Halcon vapor phase oxidation process without affecting selectivity

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carbonylation route is assigned a higher ORI due to

the extreme reaction conditions when compared to the
low-pressure carbonylation route. Use of low pressure is
recommended for high-pressure carbonylation process and
use of vapor phase reaction is recommended for liquid
phase carbonylation process. The ethanol oxidation route
is identified to be the inherently safest route as it involves
milder conditions and safer chemicals when compared to
the other routes. Sample results from the qualitative analysis of the Halcon vapor phase process are shown in Table 8.
Due to the space constraints, the complete results for the
other processes are not presented here and the reader is
referred to Palaniappan [19].

4. Conclusions
Integration of safety analysis at each design stage is vital for chemical process industries. In this paper, we have
described a systematic methodology for inherent safety
analysis during route selection stage and illustrated it using
different processes for producing acetic acid. This methodology has been implemented as one of the modules in iSafe,
an intelligent system that automates inherent safety analysis. Other modules in iSafe perform safety analysis during
product specification stage and flowsheet development. The
generic nature of the methodology in iSafe enables it to
be applicable to a variety of processes. This has been established by testing it on several case studies including acrylic
acid flowsheet development and phenol production process
routes. iSafe is envisioned to assist plant designers in developing an inherently safer chemical process. Specifically, it
would increase the awareness of the design team regarding
downstream safety consequences of early decisions on the
final design, facilitate fast track prototyping, and reduce
the time and effort spent in safety analysis at later stages.
It could thus form a part of concurrent engineering support tools for process design. iSafe can also be linked to
a database of real-life cases that provide specific examples
of inherently safer design and illustrate the synergies and
tradeoffs between safety, health, environmental aspects,
economics, and the operability of a chemical plant. We are
currently developing such as database to complement iSafe.

653

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