Relief Design for Laboratories and Pilot Plants
Jennifer F. Mize
Eastman Chemical Company, Kingsport, TN; jfmize@eastman.com (for correspondence)
Published online 5 October 2012 in Wiley Online Library (wileyonlinelibrary.com). DOI 10.1002/prs.11521
Relief designs for laboratories and pilot plants present
unique challenges to the relief designer. For example, the
relief designer must consider the need for operational flexibil-
ity while designing a relief system that provides protection for
current and future modes of operation. Therefore, small-scale
relief designs must address a wider range of potential over-
pressure scenarios due to the variations in chemistry that are
routinely conducted within the laboratory or pilot unit. The
small scale of laboratory and pilot plant operations present a
significant challenge to the relief designer in selecting and
designing effective relief systems. This article gives informa-
tion for designing laboratory and pilot plant relief systems
including: identification of relief scenarios, sizing calcula-
tion methods, relief devices, effluent discharge designs, and
other protective system considerations. Ó 2012 American Institute
of Chemical Engineers Process Saf Prog 32: 25–27, 2013
Keywords: reliefs; laboratories; pilot plants
INTRODUCTION
Relief evaluation and system design for laboratories and
pilot plants presents unique challenges to the relief designer.
Relief devices designed for commercial production-sized pro-
cess vessels are often impractical for use in laboratory and
pilot plant environments due to their size. However, typical
laboratory-scale relief devices present limitations in relieving
capacity, functionality, and available set pressures that can
make them unsuitable for many applications. Effective small-
scale relief system design must therefore also address a wider
range of potential overpressure scenarios due to the varia-
tions in chemistry that are routinely conducted within the
laboratory or pilot unit. The relief designer must consider the
need for operational flexibility while designing a relief sys-
tem that provides protection for current and future modes of
operation.
CHARACTERISTICS OF TYPICAL LABORATORY AND PILOT PLANT VESSELS
Laboratory units are typically composed of metal and
glass vessels, and glass, metal or plastic tubing and associ-
ated fittings. Each component brings unique challenges to
relief design.
Glass vessels are normally limited to use in vacuum or
low pressure operation. Glass is desirable for its transparency
and suitability for use with a wide variety of chemicals. How-
ever, even minor damage such as chips or scratches may
cause glassware to fail at a pressure much lower than the
original design pressure. Thermal shock due to temperature
changes caused by rapid heating and/or cooling can also
result in failure. Guidance may be provided by the manufac-
turer as to the design pressure rating for glass vessels. How-
ever, variations in the manufacturing process can occur
Ó 2012 American Institute of Chemical Engineers
Process Safety Progress (Vol.32, No.1)
resulting in differences in the actual pressure rating from the
target. A loose joint does not have a measured relief area nor
a tested pressure at which it will open and allow venting.
The relief designer may be unable to determine if sufficient
relief capacity can be provided by this practice to avoid
exceeding the failure pressure of the glassware.
Metal vessels and tubing allow operation at high pres-
sure (~10,000 psig). The pressure rating for such equipment
is generally available and well documented. Due to the
small size of the vessels and tubing (thick walled to allow
high pressure rating), the available relief area may be lim-
ited by the small size of nozzles and connections. However,
if the potential relief scenarios and associated overpressure
are well known, a passive solution such as selecting the
system pressure rating to exceed the maximum possible
pressure that can be generated may be the most practical
alternative.
Pilot plant units are typically constructed using metal
vessels, tubing, and piping. Vessels greater than 5 ft3 in in-
ternal volume and rated above 15 psig are generally
designed per ASME Code, Section VIII (Code) [1], much like
a full-scale production facility. Relief system design require-
ments are set by the Code for these vessels. Vessels rated
below 15 psig and small vessels (less than 6 in diameter)
are not covered by ASME Code. Drums may be used as
feed and product vessels in the pilot plant. Drums do not
have a pressure rating as they are not intended to contain
pressure. An open vent must be provided for drums that
are equipped with a nitrogen purge and/or heated to
ensure that pressure does not accumulate.
IDENTIFICATION OF RELIEF SCENARIOS/OVERPRESSURE SCENARIOS
Overpressure is defined as the accumulation of pressure
inside a vessel above its rated or maximum allowable
working pressure (MAWP). This accumulated pressure can
cause vessel failure and release of the contents to the sur-
rounding area. These scenarios are typically referred to as
relief cases, because the overpressure that is generated is
typically relieved by devices designed to prevent vessel fail-
ure (relief devices). In order to determine the credible relief
scenarios for each vessel or vessel system in the laboratory
or pilot plant unit, the relief designer must obtain, at a min-
imum, the following information: (1) vessel pressure rating,
(2) process description/process flow diagram, (3) process
chemistry, including relevant calorimetry data and cleaning
materials, (4) supply pressure for all feeds, and (5) supply
pressure and temperature for all utilities. The designer will
review this information to identify upset conditions that could
result in overpressure. The following overpressure scenarios
should be evaluated for each vessel or system. A more com-
plete discussion of these relief scenarios can be found in ANSI/
API Standard 521, Pressure Relieving and Depressuring Sys-
tems [2].
March 2013 25
1. Closed vessel outlet 9. Abnormal heat input
2. Loss of cooling 10. Split exchanger tube
3. Top reflux failure 11. Hydraulic expansion
4. Sidestream reflux failure 12. Chemical reaction
5. Noncondensable accumulation 13. External fire
6. Introduction of volatiles 14. Power failure
7. Vessel overfilling 15. Deflagration
8. Automatic control failure 16. Vacuum relief
Due to the experimental and preliminary nature of the
processes being investigated in laboratories and pilot plants,
the chemists and engineers responsible for operating the
laboratory and piloting units may not have experience with or
data for process upsets that might result in relief scenarios. This
can be a significant concern where the potential for exothermic
chemical reaction and/or thermal decomposition may result in
significant pressure and temperature increases. Additionally,
tendencies for materials in the system to plug or freeze and
potentially compromise the relief devices must be identified.
Closing recycle loops in piloting units may result in conditions
that were not previously identified in laboratory work. It may
be possible for the accumulation or production of byproducts
or waste materials to lead to additional relief scenarios.
The relief designer can identify most nonreactive relief
scenarios with basic information about the feeds and utilities.
Once the credible relief cases have been identified, the de-
signer will need to determine the maximum feed and energy
input rates in order to size the relief system. Relief for exter-
nal fire should be provided where there is sufficient fuel
(flammables and combustibles) to sustain a pool fire.
In order to determine if there are reactive relief scenarios,
the designer must obtain information from the process
experts. Differential scanning calorimetry or other thermal
testing may be necessary. Data collected in the laboratory or
piloting units are most likely geared toward developing a
process that achieves the desired products; that is, experi-
ments are not generally conducted to identify hazards due to
contamination or misoperation, or to determine safe operat-
ing limits. The following questions should be answered in
order to identify all potential reactive relief concerns:
1. Are any of the main and side reactions highly exothermic?
2. Are there any decomposition reactions or thermal instabilities?
3. What impurities are incompatible with the process (consider
utilities, seal fluids, cleaning materials, changovers, etc.)?
4. Is a runaway reaction possible?
5. How sensitive are the reaction kinetics (main and side
reactions) to the operating conditions?
6. How stable are the reactants and products and other
materials?
7. What are the consequences of an overcharge or under-
charge of one or more of the materials?
SIZING CALCULATIONS
Once the relief scenarios have been identified, the de-
signer must use sizing calculations for all credible relief
cases. Relief devices for pressure vessels (MAWP >15 psig)
should be sized in accordance with ASME Code [1], API RP
520 [3], and API RP 521[2]. All pressure relief devices (except
conservation vents) for low pressure and atmospheric vessels
(MAWP  15 psig) should be sized using the subcritical flow
correlations detailed in API RP 520, Part I [3]. Conservation vents
and vacuum relief devices should be sized using API Standard
2000 [4]. Reactive reliefs should be evaluated using Design Insti-
tute for Emergency Relief Systems methodology [5].
Sizing calculations should be documented and archived
with other process safety information for the laboratory and
pilot plant facilities. The documentation should include an
26 March 2013 Published on behalf of the AIChE
analysis of all credible relief cases, required orifice area cal-
culations, and piping system evaluations.
RELIEF DEVICES
Relief valves are spring-loaded pressure relief devices that
open at a specified set pressure and automatically reclose
when the pressure excursion ends. ASME Code relief valves
are available with set pressures ranging from 15 to 6,000
psig. These relief valves are available in sizes as small as 0.5"
3 0.75". A typical 0.5" 3 0.75" relief valve is~7 inches tall and
weighs 3 pounds, which may be too large to be used for ves-
sels in a laboratory unit. Code relief valves, however, are rou-
tinely used in pilot plant units.
Non-Code relief valves for use in laboratories and on
small pilot plant equipment are available with a wider range
of set pressure than Code relief valves. These relief valves
are available to fit standard tubing as small as 1/8". However,
these relief valves provide very small relief capacity and may
not provide adequate relief capacity for all relief scenarios. A
good example of this is a regulator failure on a high pressure
(2,000–3,000 psig) gas cylinder that allows high pressure gas
to enter downstream equipment with a low pressure rating,
such as glass equipment. The required relief area for this sce-
nario is typically an order of magnitude greater than can be
provided by a relief valve sized to fit standard tubing. How-
ever, the installation of a Code relief valve on a system con-
structed of 1/8" tubing or glass vessels may require significant
modifications to support the relief valve.
Rupture disks are nonreclosing pressure relief devices that
can be used alone or in combination with a relief valve. They
are used alone when it is desirable to keep the relief line open
after the disc has ruptured. There are limited applications for
low burst pressures (<15 psig). Rupture disks are available in
very small sizes (as small as 0.25"). The small size of the disks
results in a very high minimum burst pressure, especially for
0.25" disks such as those typically used on high pressure auto-
claves and similar vessels. For laboratory equipment, the use of
rupture disks is limited to systems with a significant pressure rat-
ing (>200 psig). Rupture disks can be a good option for pilot
plant equipment, since the available relief area for a small (1" or
2") disk is much larger than the orifice area in a relief valve with
the same size inlet connection. Additionally, since a rupture
disk is a nonreclosing device, the vessel pressure will decrease
during the relief event rather than maintaining the vessel at the
relief pressure as occurs with a relief valve. This is especially im-
portant when dealing with reactive relief scenarios.
Conservation vents are reclosing devices used for low pres-
sure applications (settings from 0.5 oz/in2 to 15 psig). They
can be used for emergency pressure relief, vacuum relief, and/
or normal breathing. Conservation vents are typically used on
large, low pressure storage tanks, and other low pressure ves-
sels (<15 psig). They are available in sizes from 2 to 24 inches
in diameter. They are generally too large to be used on labora-
tory units but may be successfully used on pilot plant equip-
ment large enough to accommodate the required nozzle size.
There are no low pressure vents designed for laboratory
units. Laboratory units typically breathe through pressure
control valves or open vents such as the discharge on vac-
uum systems. Since these are not specifically designed to
provide pressure relief, they may not be as reliable as a relief
device. The relief designer, in this case, should consider if
additional layers of protection are required to ensure labora-
tory units are properly protected.
EFFLUENT DISCHARGE AND HANDLING
For equipment located within a hood, the discharge
should be directed toward the back of the hood so that
vapors can be vented outside of the building. If liquid dis-
charge could occur, adequate drainage and splash protection
DOI 10.1002/prs Process Safety Progress (Vol.32, No.1)
should be provided, or a containment vessel should be used
so that liquid does not spill out the front of the hood.
Relief device discharges should be routed outside of the
building. The safe discharge location must be identified for
each individual relief device. In order to determine what
constitutes a safe discharge location, the toxicity, flammabil-
ity, and volatility of the material(s) involved must be consid-
ered. Both OSHA 1910.106 [6] and NFPA 30 [7] refer to dis-
charging to a ‘‘safe location.’’ OSHA 1910.106 is essentially
the 1971 version of NFPA 30. Since the regulations do not
provide prescriptive information on discharging to a ‘‘safe
location,’’ documents such as API 521 and books such as
Guidelines for Pressure Relief and Effluent Handling [5], pub-
lished by the Center for Chemical Process Safety of the Amer-
ican Institute of Chemical Engineers, provide good engineer-
ing practice for the design of relief systems. 29 CFR 1910.119
Appendix C, Section 3 (part of the OSHA PSM Standard) [8]
provides additional sources for good engineering practices.
The discharge piping layout for relief systems must adhere
to the following criteria in order to provide a reliable and
safe system:
• Provide a proper and safe path for relieving fluids
• Have a maximum pressure drop of 10% of the set pres-
sure of conventional relief valves (not applicable to rup-
ture discs or conservation vents; value for balanced bel-
lows valves will vary)
• Account for backpressure (both static and dynamic) and
pressure interaction with other piping and vessels con-
nected to the system
• Account for material of construction relationships with
other piping in the system
• Account for relief device maintenance requirements
Secondary containment means, such as blowdown tanks
and vent stack systems should be designed to handle credi-
ble simultaneous relief flows from connected equipment.
Due to the wide variety of process chemistry that may be
handled in pilot plant units, compatibility concerns created
by discharging multiple unit reliefs into a common vessel
may exist and should be addressed as part of the relief
design effort. A single effluent handling system for a pilot
plant complex may not provide an acceptable discharge loca-
tion for all units depending upon the chemicals present.
OTHER PROTECTIVE SYSTEMS
One approach is to design the vessels to eliminate or miti-
gate as many potential relief scenarios as possible. The ex-
pectation that various chemistries will be run within the
equipment during the service life of the laboratory or pilot
unit makes it even more important to consider selecting the
maximum practical pressure rating for all vessels in the sys-
tem as part of the equipment design. Normal operating pres-
sure and temperature should never be used as the basis for
specification of the vessel pressure rating. Increasing the
pressure rating decreases the required relief area and relief
device size and may eliminate relief scenarios. Laboratory
and small pilot plant equipment can be shielded by the use
of barriers or high pressure cubicles. Providing this type of
protection for personnel does not eliminate the need for
adequate pressure relief in all installations but can serve as
an additional layer of protection against personnel injury.
Process Safety Progress (Vol.32, No.1) Published on behalf of the AIChE
The use of fire resistant insulation is highly recommended
for all pilot plant vessels. Fire resistant insulation not only
provides mitigation for relief sizing for external fire impinge-
ment, but it also increases the time required to heat the
materials in the vessel to the relief conditions.
CONCLUSION
Effective relief system design for laboratories and pilot
plants is essential to ensure safe operation of the facilities.
The small scale of laboratory and pilot plant vessels presents
a challenge to the relief designer in selecting an effective
relief system design. Identification of credible relief scenarios
requires an assessment of both reactive and nonreactive haz-
ards to ensure a robust relief system design. Other safety
measures such as the use of inherently safer design, physical
barriers, and fire protection can be used in place of or in
addition to a properly designed relief system.
A more detailed article concerning this topic was pre-
sented in the Global Congress [9]. There are also a couple of
other PSP articles that will help laboratories and pilot plants
improve their safety in relationship to relief designs [10, 11].
LITERATURE CITED
1. American Society of Mechanical Engineers, Boiler and
Pressure Vessel Code (BPVC), Section VIII, Division 1,
ASME, New York, NY, 2010
2. ANSI/API Standard 521, Pressure Relieving and Depressur-
ing Systems/ISO 23251, Petroleum, Petrochemical, and
Natural gas Industries—Pressure-Relieving and Depressur-
ing Systems, American Petroleum Institute, Washington, DC,
2007.
3. American Petroleum Institute, API RP 520: Sizing, Selection,
and Installation of Pressure-Relieving Devices in Refineries,
American Petroleum Institute, Washington, DC, 2000.
4. American Petroleum Institute, API (2000): Venting Atmos-
pheric and Low-Pressure Storage Tanks, American Petroleum
Institute, Washington, DC, 1998.
5. Center for Chemical Process Safety (CCPS), Guidelines
for Pressure Relief and Effluent Handling Systems,
Wiley-AIChE, New York, NY, 1998.
6. Occupational Safety & Health Administration, U.S. Depart-
ment of Labor, Occupational Safety and Health Standards:
1910.106, Flammable and Combustible Liquids, OSHA, Wash-
ington, DC, 1976.
7. National Fire Protection Association, NFPA 30: Flammable
and Combustible Liquids Code, NFPA, Quincy, MA, 2012.
8. Occupational Safety & Health Administration, U.S. Depart-
ment of Labor, Occupational Safety and Health Standards:
1910.119, Process Safety Management of Highly Hazard-
ous Chemicals, OSHA, Washington, DC, 1996.
9. J.F. Mize, Relief design for laboratories and pilot plants,
Proceedings of the AIChE Spring Meeting & 8th Global
Congress on Process Safety, Houston, Texas, paper 79c,
2012.
10. R.N. Brummel, Procedures for preventing pilot plant run-
aways, Plant/Oper Prog 8 (1989), 228–233.
11. R.P. Palluzi, Performance analysis of small size pilot plant
and laboratory relief valves, Process Saf Prog 22 (2003),
137–140.
DOI 10.1002/prs March 2013 27