Safety

Properly Purge and

Inert Storage Vessels
George R. Kinsley, Jr.,
Environmental Resources
Management, Inc.

Inert gases are used

P urging and inerting (or blanketing) process vessels and
equipment are two common, yet distinctive, practices to
control the concentration of oxygen, thereby reducing
fire and explosion hazards. Purging usually refers to the
short-term addition of an inert gas (e.g., nitrogen or carbon dioxide)
to a tank, process vessel, or other piece of process equipment that
contains flammable vapors or gases to render the space nonignitable
for a specific time period (say, during a maintenance outage). In con-
to prevent fires trast, inerting (or blanketing) is the long-term maintenance of an
and explosions in inert atmosphere in the vapor space of a container or vessel during
operation.
the vapor spaces
of equipment. Safe oxygen levels
The goal of these methods is to reduce a vessel’s oxygen concen-
Correct selection tration below the limiting oxygen concentration (LOC). The LOC is
the concentration of oxidant below which a deflagration cannot
of the oxygen occur in a specified mixture. The LOCs for common flammable
concentration and gases and vapors, using a nitrogen or carbon dioxide diluent, are list-
ed in Table 1. A safety margin must be maintained between the LOC
the inert gas-flow and the normal working concentration in the system. Conservative
rate are critical to control typically uses 2–4 percentage points below the LOC. That is,
if the LOC of ethanol using nitrogen as a diluent is 10.5%, the con-
ensuring safety. trol point would be 6.5–8.5%.
Although nitrogen or carbon dioxide are the most common inert-
< Discuss This Article! > ing gases, steam is sometimes used. If so, it must be supplied at a rate
sufficient to maintain the vessel temperature at 160°F or higher and
To join an online discussion about this article
with the author and other readers, go to the
care must be taken so that condensation by cooling does not draw in
ProcessCity Discussion Room for CEP articles atmospheric air or collapse the vessel by implosion (1).
at www.processcity.com/cep. This temperature is experience-based and is considered sufficient to
prevent condensation of the steam, which would hinder the protection

CEP February 2001 www.aiche.org/cep/ 57

Safety

to the vessel from the steam purge. Table 1. LOCs for selected gases and vapors.
Possible sources of purge or inert-
ing gases include commercially avail- Gas or Vapor LOC for N2/Air LOC for CO2/Air
able gases supplied from high-pres- O2, vol. % O2, vol. %
sure cryogenic tanks or standard
Cyclopropane 11.5 14
cylinders, or on-site air separation Natural gas (Pittsburgh) 12 14.5
plants that remove oxygen from the n-butyl chloride 14 —
Acetone 11.5 14
air and recover nitrogen by liquefac- Carbon disulfide 5 7.5
tion followed by absorption, chemical Ethanol 10.5 13
reaction, or membrane permeation. Hydrogen 5 5.2
Methyl ether 10.5 13
Cross-connections between the Methyl ethyl ketone 11 13.5
source of inerting gas and any other
Source: Adapted from Ref. 3.
system should not be allowed. The
gases from an enclosure or vessel
being purged must be vented at a safe pump). The steps in a vacuum purge Solution:
location. The purging or inerting gas are: (1) drawing a vacuum on the ves- xo = 0.21 lb-mole O2/total moles
should be introduced and exhausted sel until the desired level is achieved; The number of purge cycles k is
so that effective mixing is ensured (2) relieving the vacuum with an inert determined by rewriting Eq. 1 to
and the desired reduction in oxidant gas such as nitrogen to atmospheric solve for k (2):
concentration is maintained through- pressure; and (3) repeating Steps 1 and
out the system being protected. Mul- 2 until the desired oxygen concentra- x
tiple inlets and outlets are desirable to tion is reached. The amount of purge ln x k
o
promote diluent distribution. gas required depends upon the number k= (3)
PL
Several methods may be used to of evacuations needed to develop the ln
PH
form and maintain a noncombustible desired oxygen concentration.
atmosphere in an enclosure. These in- The oxygen concentration x after k
clude batch modes for one-time use, purge cycles (vacuum and relief) is Substituting in (2):
such as purging equipment during a described by Eq. 1, assuming that the
shutdown, and continuous inerting to pressure limits PH and PL are identi-
assure safe conditions during normal cal for each cycle (2): ln 0.02
0.21
operations. Each method will be de- k= = 0.69 or 1 cycle (4)
scribed and illustrative sample design ln 25
k 760
calculations will be made. PL
xk = xo (1)
PH
Syphon and vacuum purging The total nitrogen used is deter-
The common batch purging meth- The quantity of inert gas required mined from Eq. 2 (1):
ods are syphon, vacuum, pressure, may be calculated by Eq. 2 for k cy-
and sweep-through. cles, based on the ideal gas law (2): P2 – P1
Syphon purging involves filling the V2 = V1 (5)
P2
vessel to be purged with liquid (i.e., PH – PL V1
product or water) followed by intro- V2 = k (2)
PH
ducing the purge gas, typically nitro-
gen, into the vapor space as the liquid V2 = 760 – 25 5,000 gal ×
760
is drained. The required purge-gas vol- Example 1: Determine the number
ume equals the volume of the vessel. of purges required and the total con-
The rate of application corresponds to sumption of nitrogen to reduce the 1 ft 3/7.48 gal = 646.5 ft 3 (6)
the volumetric rate of liquid discharge. oxygen concentration in a 5,000 gal
Syphon purging may not be appropri- tank to 2% before introducing ace- or 1.66 lb-mol.
ate if the liquid is above its flashpoint tone. The temperature is 75°F and the
due to evaporation into the space. vessel is initially charged with air at Pressure purging
Vacuum purging is one of the most atmospheric pressure. A steam ejector Vessels may also be purged by
common vessel inerting procedures is used that reaches 25 mm Hg abso- adding inert gas under pressure and,
provided that the vessel is designed for lute and the vacuum of each cycle is after the gas has sufficiently diffused,
the maximum vacuum that can be de- relieved with pure nitrogen until the venting to atmosphere. As with vacu-
veloped by the source (e.g., a vacuum pressure equals 1 atm. um purging, more than one pressure

58 www.aiche.org/cep/ February 2001 CEP

 ■ Figure 1. The relationship between the number
1.0 Dilution ratio of volumes of oxygen-free purge gas
for purging
at atmospheric
(e.g., nitrogen) that enters the vessel
Fraction of Original Concentration

0.8 pressure, and the reduction in the vessel’s oxy-

assuming gen concentration, assuming complete
complete mixing. mixing, is shown in Figure 1 (3).
0.6 An oxygen material balance
around the vessel is (2):
0.4
V dc = C oQ – CQ (11)
dt
0.2
Equation 11 can be rearranged and
0
integrated, assuming Co = 0 (2):
0 1 2 3 4 5 6
t C2
Number of Volumes of Purge Gas Injected dc
Q= dt = V c (12)
o C1

cycle may be necessary to reduce the ln 0.01 Integrating Eq. 12 yields Eq. 13, the
concentration of oxygen to the desired 0.03 volumetric flow rate required to reduce
k= = 0.54 (9)
level. The mathematical relationship ln 14.7 the vessel’s oxygen concentration from
that describes the pressure purging 114.7 C1 (initial condition) to C2 (2):
process is identical to Eq. 1, except
that the initial concentration of oxy- Thus, the number of purge cycles C1
gen in the vessel xo is computed after = 1, and the nitrogen consumption is Qt = V ln (13)
C2
the vessel is initially pressurized. calculated as follows:
Example 2: Determine the number
of nitrogen pressure purges required 100 – 14.7 – 14.7 Equation 13 assumes perfect mix-
and the total consumption of nitrogen V2 = × ing. Since this is not normally the
needed to reduce the oxygen concen- 100 + 14.7 case in actual practice, a correction
tration in the 5,000 gal tank described 5,000 gal = 582.8 ft 3 factor K is used. Table 2 lists values
in Example 1 to 1% oxygen. The ni- of K for certain conditions. Since lit-
trogen is supplied to the vessel at 100 or 11.65 lb–mole (10) tle data exist on defining the degree
psig and 75°F. of mixing, conservatism recommends
Solution: Equation 1 is used to de- a value of K no greater than 0.25.
termine the number of purge cycles. Note the increased consumption Equation 13 then becomes (3):
The initial oxygen concentration in the compared to vacuum purging (Exam-
vessel is calculated after the first pres- ple 1), because the vessel must be pres- C
surization using a simple pressure ratio surized to 100 psig during each cycle. Qt = V ln 1 (14)
K C2
where PL is the starting or atmospheric
pressure, whichever is appropriate. Sweep-through purging
This method introduces a purge Example 3: A 20,000 gal storage
P gas into a vessel at one opening and vessel that contains 100% air must be
xo = 0.21 L (7) withdraws the mixed gas at another inerted with nitrogen until the oxygen
PH
opening and vents it to the atmo- concentration is 2% by volume. How
sphere (or an air-pollution control-de- much nitrogen must be swept
14.7 psia vice), thus, sweeping out residual through? Assume K = 0.25.
xo = 0.21 flammable vapor. The quantity of
100 psia + 14.7 psia
purge gas required depends upon the Solution: The volume
20,000 gal of nitrogen
1 ft 3
physical arrangement. Sweep-through Qt =
required Qt is ln 0.21 ×
determined by Eq. 14:
(8) 0.25 0.02 7.48 gal
= 0.03 lb–mole purging is commonly used when the
vessel is not rated for pressure or vac-
= 25,148 ft 3 N 2 or 9.41 air changes
Applying Eq. 1, the number of cy- uum. The purge gas is introduced and
cles is: withdrawn at atmospheric pressure. (15)

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Safety
Table 2. Mixing efficiencies for selected
ventilation arrangements.
Single Exhaust Multiple Exhaust
Source of Supply Opening
Infiltration through cracks, open 0.2
doors, or windows
Powered air supply through:
• Grills and registers 0.3
• Diffusers 0.5
• Perforated ceilings 0.8
• Pipes and ducts 0.25*
* Conservative recommendation based on NFPA 69 (3).
Inerting
Continuous inerting methods are
fixed- and variable-rate (or demand).
Fixed-rate application involves con-
tinuous feeding of inert gas into an
enclosure (e.g., vessel) at a constant
rate and the corresponding release of
a mixture of inert gas and flammable
vapor that has been picked up in the
vessel’s headspace. To ensure that the
vessel is completely protected, the
rate must be sufficient to satisfy
peak-demand requirements.
The peak demand for continuous
inerting is typically controlled by the
maximum liquid withdrawal rate
coupled with potential temperature
changes. For a vessel containing a
flammable liquid, the inert gas de-
mand based on liquid withdrawal is
the capacity of the largest pump used
to withdraw liquid or the maximum
possible gravity outflow rate,
whichever is greater.
The maximum demand from a
temperature change will occur in out-
door tanks operating at or near atmo-
spheric pressure as a result of the
sudden cooling from a summer thun-
derstorm. The rate of inert gas neces-
sary to prevent the vessel’s pressure
from falling significantly below at-
mospheric pressure is determined as
follows: (1) for tanks over 800,000
gallons capacity, 2 ft3/h of inert gas
per square foot of tank surface (shell
and roof); and (2) for smaller tanks, 1
ft3/h of gas per 40 gal of tank capaci-
ty. Optionally, an inert gas rate corre-
60 www.aiche.org/cep/ February 2001
From N2
Distribution
Header
Efficiency, K
Openings
Strainer
0.3–0.4
0.5 Orifice Plate–
0.7
0.9 Sized Based on
0.25* Peak Demand
■ Figure 2.
One method of flow
control for a fixed-rate Drain
application.
sponding to the mean rate of change
of the vapor-space temperature of
100°F/h may be used. The rates cor-
responding to a temperature change
and liquid withdrawal must be added
together to determine the peak rate.
These numbers are experience-based
and are found in Refs. 1 and 3.
Variable rate or demand inerting
involves feeding inert gas into the
vessel at a rate that is a function of
demand. Demand is based on main-
taining a pressure within the vessel
that is slightly above that of the sur-
rounding atmosphere (e.g., ~1 in.
H2O).
Variable application offers an ob-
vious advantage over continuous in
that inert gas is supplied only when it
is actually needed, thereby reducing:
(1) the total quantity of inert gas re-
quired; (2) product loss; and (3) dis-
posal problems. A disadvantage is
the dependence upon flow control de-
vices actuated by very low pressure-
differentials that are sometimes diffi-
cult to maintain.
For variable-rate application, an
inerting system is required to main-
tain such an atmosphere in the vapor
space above the liquid. Ideally, this
system should include an automatic
inert-gas addition valve or backpres-
CEP
Alarm for High
O2 Concentration
A
O2 Analyzer
in Vessel
Vapor Space
Check
Valve
Styrene
Monomer
To
Process
Storage Tank
Containing Styrene
Monomer
sure regulator to control the oxygen
concentration below the LOC. The
control system should feature an ana-
lyzer to continuously monitor the
oxygen concentration and allow inert
gas to enter the space to maintain the
oxygen concentration at safe levels
with a reasonable margin of safety.
An increase in the concentration
above the set point should initiate an
alarm and shut down the operation.
Where the oxygen concentration can-
not be continuously monitored, it
should be designed to operate at no
more than 60% of the LOC and
checked on a regularly scheduled
basis.
Figure 2 shows one simple
method of flow control that can be
used with a continuous introduction
of purge gas. Figure 3 depicts a
method than can be used with vari-
able rate application.
Practical considerations
Operation of a system with an
oxygen concentration low enough to
prevent a deflagration does not nec-
essarily mean that incipient fires are
absolutely prevented. Smoldering
can occur in fibrous materials at low
oxidant concentrations, later result-
ing in a fire or explosion when ex-
 ■ Figure 3. upset a reaction or cause exhaust sys-
From N2 Typical setup for
Distribution tem damage. The flowing gas will
flow control in a
Header
variable-rate
also carry volatile materials (sol-
application. vents) from the vessel. Consider
O2 Analyzer
what these materials will do in the
in Vessel exhaust system. Traps, filters, or ab-
S Strainer
Vapor Space sorbers may be necessary to treat the
exhaust.
Finally, there can be no doubt that
Flow Control Check without nitrogen (or other inert gas)
Valve, Size Valve purging and inerting, many more peo-
S
Based on ple would be injured or killed by fire
Peak Demand
and explosion. Nevertheless, we have
Styrene paid a heavy price for the benefits of
Monomer nitrogen. Many employees have been
Solenoid S
Valves asphyxiated by it. During the period
To
Storage Tank Process
from 1960 to 1978, one group of
Containing Styrene companies reported that 13 employ-
Drain Monomer ees were killed by fire or explosion,
13 by toxic or corrosive chemicals,
and 7 by nitrogen.
posed to a higher concentration. The • Operating controls; If a person enters an atmosphere
physical and chemical properties of • Maintenance, inspection, and of nitrogen, he or she can lose con-
the flammable or combustible materi- testing; sciousness without any warning
als involved will govern the type and • Leakage of purge gas to sur- symptoms in as little as 20 s. Death
required purity of the purge gas rounding areas; and can follow in 3–4 min. A person falls
needed. • Need for breathing apparatus by as if struck by a blow on the head. In
The following factors should be personnel. one incident in which the author was
considered in the design of any sys- The minimum achievable oxygen involved, a viewing hatch in a vessel
tem to reduce the oxidant concentra- concentration will depend upon the containing vegetable oil was re-
tions to safe levels: purity of the inert gas, the vessel’s moved, but the nitrogen was kept
• Required reduction in oxidant gas-tight integrity, and the presence of flowing to protect the material from
concentration; back diffusion from the exhaust line. oxidation. A supervisor did not ask
• Variations in the process, pro- To maintain a given oxygen concen- for an entry permit as he intended
cess temperature and pressure, and tration, it may be necessary to contin- only to peek in. Fortunately, someone
materials being processed; ue to supply inert gas even after at- noticed that he was no longer moving
• Purge gas supply source and tainment of the desired oxygen level. and he was rescued in time. Whenev-
equipment installation; Flowing inert gas will remove er nitrogen (or other asphyxiating
• Compatibility of the purge gas heat from the vessel (e.g., a heated gas) is used for inerting or purging,
with the process; reactor or oven). Care should be employee training, strict adherence to
taken that this heat removal will not a confined space entry procedure and
Nomenclature permit system, and vessel labeling are
a must. CEP
C = concentration of oxygen in the vessel Literature Cited
Co = inlet oxygen concentration (0, when
inerting with nitrogen) 1. “Inerting and Purging of Tanks, Process
k = number of purge cycles Vessels, and Equipment,” Factory Mutu- G. R. KINSLEY, Jr. is principal-in-charge and
K = correction factor in Eq. 14 for degree of safety and health practice area leader
mixing
al Loss Prevention Data Sheet 7-59, Fac-
for Environmental Resources Management,
PH, P2 = initial high or atmospheric pressure tory Mutual Engineering Corp., Nor-
Inc., Vernon Hills, IL ((847) 680-6868;
PL, P1 = initial vacuum pressure wood, MA (1977). Fax: (847) 680-6847; E-mail:
V = vessel volume 2. Crowl, D. A., and J. F. Louvar, “Chem- george_kinsley@erm.com). He has
Q = volumetric flow rate of inerting gas
t = time
ical Process Safety — Fundamentals served in the U.S. Army Corps of Engineers,
V1 = total volume of tank or enclosure With Applications,” Prentice Hall, Upper and is a Certified Safety Professional,
V2 = volume of inert gas required, measured at Saddle River, NJ, pp. 195–200 (1990). a U.S. patent holder, and a professional
PH 3. “Standard on Explosion Prevention Sys- member of the American Society of Safety
xk = final oxygen concentration after k purge Engineers. He holds a BSChE from Drexel
cycles
tems,” NFPA 69, National Fire Prevention
University and an MBA from Widener
xo = initial oxygen concentration under vacuum Association, Quincy, MA (1997 edition).
University (Chester, PA).

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