Relief Design for Laboratories and Pilot Plants

Jennifer F. Mize
Eastman Chemical Company, Kingsport, TN; [email protected] (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 resulting in differences in the actual pressure rating from the
unique challenges to the relief designer. For example, the target. A loose joint does not have a measured relief area nor
relief designer must consider the need for operational flexibil- a tested pressure at which it will open and allow venting.
ity while designing a relief system that provides protection for The relief designer may be unable to determine if sufficient
current and future modes of operation. Therefore, small-scale relief capacity can be provided by this practice to avoid
relief designs must address a wider range of potential over- exceeding the failure pressure of the glassware.
pressure scenarios due to the variations in chemistry that are Metal vessels and tubing allow operation at high pres-
routinely conducted within the laboratory or pilot unit. The sure (~10,000 psig). The pressure rating for such equipment
small scale of laboratory and pilot plant operations present a is generally available and well documented. Due to the
significant challenge to the relief designer in selecting and small size of the vessels and tubing (thick walled to allow
designing effective relief systems. This article gives informa- high pressure rating), the available relief area may be lim-
tion for designing laboratory and pilot plant relief systems ited by the small size of nozzles and connections. However,
including: identification of relief scenarios, sizing calcula- if the potential relief scenarios and associated overpressure
tion methods, relief devices, effluent discharge designs, and are well known, a passive solution such as selecting the
other protective system considerations. Ó 2012 American Institute system pressure rating to exceed the maximum possible
of Chemical Engineers Process Saf Prog 32: 25–27, 2013 pressure that can be generated may be the most practical
Keywords: reliefs; laboratories; pilot plants alternative.
Pilot plant units are typically constructed using metal
vessels, tubing, and piping. Vessels greater than 5 ft3 in in-
INTRODUCTION ternal volume and rated above 15 psig are generally
Relief evaluation and system design for laboratories and designed per ASME Code, Section VIII (Code) [1], much like
pilot plants presents unique challenges to the relief designer. a full-scale production facility. Relief system design require-
Relief devices designed for commercial production-sized pro- ments are set by the Code for these vessels. Vessels rated
cess vessels are often impractical for use in laboratory and below 15 psig and small vessels (less than 6 in diameter)
pilot plant environments due to their size. However, typical are not covered by ASME Code. Drums may be used as
laboratory-scale relief devices present limitations in relieving feed and product vessels in the pilot plant. Drums do not
capacity, functionality, and available set pressures that can have a pressure rating as they are not intended to contain
make them unsuitable for many applications. Effective small- pressure. An open vent must be provided for drums that
scale relief system design must therefore also address a wider are equipped with a nitrogen purge and/or heated to
range of potential overpressure scenarios due to the varia- ensure that pressure does not accumulate.
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 IDENTIFICATION OF RELIEF SCENARIOS/OVERPRESSURE SCENARIOS
operation. Overpressure is defined as the accumulation of pressure
inside a vessel above its rated or maximum allowable
working pressure (MAWP). This accumulated pressure can
CHARACTERISTICS OF TYPICAL LABORATORY AND PILOT PLANT VESSELS
Laboratory units are typically composed of metal and cause vessel failure and release of the contents to the sur-
glass vessels, and glass, metal or plastic tubing and associ- rounding area. These scenarios are typically referred to as
ated fittings. Each component brings unique challenges to relief cases, because the overpressure that is generated is
relief design. typically relieved by devices designed to prevent vessel fail-
Glass vessels are normally limited to use in vacuum or ure (relief devices). In order to determine the credible relief
low pressure operation. Glass is desirable for its transparency scenarios for each vessel or vessel system in the laboratory
and suitability for use with a wide variety of chemicals. How- or pilot plant unit, the relief designer must obtain, at a min-
ever, even minor damage such as chips or scratches may imum, the following information: (1) vessel pressure rating,
cause glassware to fail at a pressure much lower than the (2) process description/process flow diagram, (3) process
original design pressure. Thermal shock due to temperature chemistry, including relevant calorimetry data and cleaning
changes caused by rapid heating and/or cooling can also materials, (4) supply pressure for all feeds, and (5) supply
result in failure. Guidance may be provided by the manufac- pressure and temperature for all utilities. The designer will
turer as to the design pressure rating for glass vessels. How- review this information to identify upset conditions that could
ever, variations in the manufacturing process can occur 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-
Ó 2012 American Institute of Chemical Engineers tems [2].

Process Safety Progress (Vol.32, No.1) March 2013 25

1. Closed vessel outlet 9. Abnormal heat input analysis of all credible relief cases, required orifice area cal-
2. Loss of cooling 10. Split exchanger tube culations, and piping system evaluations.
3. Top reflux failure 11. Hydraulic expansion
4. Sidestream reflux failure 12. Chemical reaction RELIEF DEVICES
5. Noncondensable accumulation 13. External fire Relief valves are spring-loaded pressure relief devices that
6. Introduction of volatiles 14. Power failure open at a specified set pressure and automatically reclose
7. Vessel overfilling 15. Deflagration when the pressure excursion ends. ASME Code relief valves
8. Automatic control failure 16. Vacuum relief 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
Due to the experimental and preliminary nature of the weighs 3 pounds, which may be too large to be used for ves-
processes being investigated in laboratories and pilot plants, sels in a laboratory unit. Code relief valves, however, are rou-
the chemists and engineers responsible for operating the tinely used in pilot plant units.
laboratory and piloting units may not have experience with or Non-Code relief valves for use in laboratories and on
data for process upsets that might result in relief scenarios. This small pilot plant equipment are available with a wider range
can be a significant concern where the potential for exothermic of set pressure than Code relief valves. These relief valves
chemical reaction and/or thermal decomposition may result in are available to fit standard tubing as small as 1/8". However,
significant pressure and temperature increases. Additionally, these relief valves provide very small relief capacity and may
tendencies for materials in the system to plug or freeze and not provide adequate relief capacity for all relief scenarios. A
potentially compromise the relief devices must be identified. good example of this is a regulator failure on a high pressure
Closing recycle loops in piloting units may result in conditions (2,000–3,000 psig) gas cylinder that allows high pressure gas
that were not previously identified in laboratory work. It may to enter downstream equipment with a low pressure rating,
be possible for the accumulation or production of byproducts such as glass equipment. The required relief area for this sce-
or waste materials to lead to additional relief scenarios. nario is typically an order of magnitude greater than can be
The relief designer can identify most nonreactive relief provided by a relief valve sized to fit standard tubing. How-
scenarios with basic information about the feeds and utilities. ever, the installation of a Code relief valve on a system con-
Once the credible relief cases have been identified, the de- structed of 1/8" tubing or glass vessels may require significant
signer will need to determine the maximum feed and energy modifications to support the relief valve.
input rates in order to size the relief system. Relief for exter- Rupture disks are nonreclosing pressure relief devices that
nal fire should be provided where there is sufficient fuel can be used alone or in combination with a relief valve. They
(flammables and combustibles) to sustain a pool fire. are used alone when it is desirable to keep the relief line open
In order to determine if there are reactive relief scenarios, after the disc has ruptured. There are limited applications for
the designer must obtain information from the process low burst pressures (<15 psig). Rupture disks are available in
experts. Differential scanning calorimetry or other thermal very small sizes (as small as 0.25"). The small size of the disks
testing may be necessary. Data collected in the laboratory or results in a very high minimum burst pressure, especially for
piloting units are most likely geared toward developing a 0.25" disks such as those typically used on high pressure auto-
process that achieves the desired products; that is, experi- claves and similar vessels. For laboratory equipment, the use of
ments are not generally conducted to identify hazards due to rupture disks is limited to systems with a significant pressure rat-
contamination or misoperation, or to determine safe operat- ing (>200 psig). Rupture disks can be a good option for pilot
ing limits. The following questions should be answered in plant equipment, since the available relief area for a small (1" or
order to identify all potential reactive relief concerns: 2") disk is much larger than the orifice area in a relief valve with
the same size inlet connection. Additionally, since a rupture
1. Are any of the main and side reactions highly exothermic? disk is a nonreclosing device, the vessel pressure will decrease
2. Are there any decomposition reactions or thermal instabilities? during the relief event rather than maintaining the vessel at the
3. What impurities are incompatible with the process (consider relief pressure as occurs with a relief valve. This is especially im-
utilities, seal fluids, cleaning materials, changovers, etc.)? portant when dealing with reactive relief scenarios.
4. Is a runaway reaction possible? Conservation vents are reclosing devices used for low pres-
5. How sensitive are the reaction kinetics (main and side sure applications (settings from 0.5 oz/in2 to 15 psig). They
reactions) to the operating conditions? can be used for emergency pressure relief, vacuum relief, and/
6. How stable are the reactants and products and other or normal breathing. Conservation vents are typically used on
materials? large, low pressure storage tanks, and other low pressure ves-
7. What are the consequences of an overcharge or under- sels (<15 psig). They are available in sizes from 2 to 24 inches
charge of one or more of the materials? 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.
SIZING CALCULATIONS
Once the relief scenarios have been identified, the de- There are no low pressure vents designed for laboratory
signer must use sizing calculations for all credible relief units. Laboratory units typically breathe through pressure
cases. Relief devices for pressure vessels (MAWP >15 psig) control valves or open vents such as the discharge on vac-
should be sized in accordance with ASME Code [1], API RP uum systems. Since these are not specifically designed to
520 [3], and API RP 521[2]. All pressure relief devices (except provide pressure relief, they may not be as reliable as a relief
conservation vents) for low pressure and atmospheric vessels device. The relief designer, in this case, should consider if
(MAWP  15 psig) should be sized using the subcritical flow additional layers of protection are required to ensure labora-
correlations detailed in API RP 520, Part I [3]. Conservation vents tory units are properly protected.
and vacuum relief devices should be sized using API Standard
2000 [4]. Reactive reliefs should be evaluated using Design Insti- EFFLUENT DISCHARGE AND HANDLING
tute for Emergency Relief Systems methodology [5]. For equipment located within a hood, the discharge
Sizing calculations should be documented and archived should be directed toward the back of the hood so that
with other process safety information for the laboratory and vapors can be vented outside of the building. If liquid dis-
pilot plant facilities. The documentation should include an charge could occur, adequate drainage and splash protection

26 March 2013 Published on behalf of the AIChE DOI 10.1002/prs Process Safety Progress (Vol.32, No.1)
should be provided, or a containment vessel should be used The use of fire resistant insulation is highly recommended
so that liquid does not spill out the front of the hood. for all pilot plant vessels. Fire resistant insulation not only
Relief device discharges should be routed outside of the provides mitigation for relief sizing for external fire impinge-
building. The safe discharge location must be identified for ment, but it also increases the time required to heat the
each individual relief device. In order to determine what materials in the vessel to the relief conditions.
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 CONCLUSION
the 1971 version of NFPA 30. Since the regulations do not Effective relief system design for laboratories and pilot
provide prescriptive information on discharging to a ‘‘safe plants is essential to ensure safe operation of the facilities.
location,’’ documents such as API 521 and books such as The small scale of laboratory and pilot plant vessels presents
Guidelines for Pressure Relief and Effluent Handling [5], pub- a challenge to the relief designer in selecting an effective
lished by the Center for Chemical Process Safety of the Amer- relief system design. Identification of credible relief scenarios
ican Institute of Chemical Engineers, provide good engineer- requires an assessment of both reactive and nonreactive haz-
ing practice for the design of relief systems. 29 CFR 1910.119 ards to ensure a robust relief system design. Other safety
Appendix C, Section 3 (part of the OSHA PSM Standard) [8] measures such as the use of inherently safer design, physical
provides additional sources for good engineering practices. barriers, and fire protection can be used in place of or in
The discharge piping layout for relief systems must adhere addition to a properly designed relief system.
to the following criteria in order to provide a reliable and A more detailed article concerning this topic was pre-
safe system: sented in the Global Congress [9]. There are also a couple of
other PSP articles that will help laboratories and pilot plants
• Provide a proper and safe path for relieving fluids improve their safety in relationship to relief designs [10, 11].
• Have a maximum pressure drop of 10% of the set pres-
sure of conventional relief valves (not applicable to rup-
LITERATURE CITED
ture discs or conservation vents; value for balanced bel-
1. American Society of Mechanical Engineers, Boiler and
lows valves will vary)
Pressure Vessel Code (BPVC), Section VIII, Division 1,
• Account for backpressure (both static and dynamic) and ASME, New York, NY, 2010
pressure interaction with other piping and vessels con-
2. ANSI/API Standard 521, Pressure Relieving and Depressur-
nected to the system
ing Systems/ISO 23251, Petroleum, Petrochemical, and
• Account for material of construction relationships with Natural gas Industries—Pressure-Relieving and Depressur-
other piping in the system
ing Systems, American Petroleum Institute, Washington, DC,
• Account for relief device maintenance requirements 2007.
Secondary containment means, such as blowdown tanks 3. American Petroleum Institute, API RP 520: Sizing, Selection,
and vent stack systems should be designed to handle credi- and Installation of Pressure-Relieving Devices in Refineries,
ble simultaneous relief flows from connected equipment. American Petroleum Institute, Washington, DC, 2000.
Due to the wide variety of process chemistry that may be 4. American Petroleum Institute, API (2000): Venting Atmos-
handled in pilot plant units, compatibility concerns created pheric and Low-Pressure Storage Tanks, American Petroleum
by discharging multiple unit reliefs into a common vessel Institute, Washington, DC, 1998.
may exist and should be addressed as part of the relief 5. Center for Chemical Process Safety (CCPS), Guidelines
design effort. A single effluent handling system for a pilot for Pressure Relief and Effluent Handling Systems,
plant complex may not provide an acceptable discharge loca- Wiley-AIChE, New York, NY, 1998.
tion for all units depending upon the chemicals present. 6. Occupational Safety & Health Administration, U.S. Depart-
ment of Labor, Occupational Safety and Health Standards:
OTHER PROTECTIVE SYSTEMS 1910.106, Flammable and Combustible Liquids, OSHA, Wash-
One approach is to design the vessels to eliminate or miti- ington, DC, 1976.
gate as many potential relief scenarios as possible. The ex- 7. National Fire Protection Association, NFPA 30: Flammable
pectation that various chemistries will be run within the and Combustible Liquids Code, NFPA, Quincy, MA, 2012.
equipment during the service life of the laboratory or pilot 8. Occupational Safety & Health Administration, U.S. Depart-
unit makes it even more important to consider selecting the ment of Labor, Occupational Safety and Health Standards:
maximum practical pressure rating for all vessels in the sys- 1910.119, Process Safety Management of Highly Hazard-
tem as part of the equipment design. Normal operating pres- ous Chemicals, OSHA, Washington, DC, 1996.
sure and temperature should never be used as the basis for 9. J.F. Mize, Relief design for laboratories and pilot plants,
specification of the vessel pressure rating. Increasing the Proceedings of the AIChE Spring Meeting & 8th Global
pressure rating decreases the required relief area and relief Congress on Process Safety, Houston, Texas, paper 79c,
device size and may eliminate relief scenarios. Laboratory 2012.
and small pilot plant equipment can be shielded by the use 10. R.N. Brummel, Procedures for preventing pilot plant run-
of barriers or high pressure cubicles. Providing this type of aways, Plant/Oper Prog 8 (1989), 228–233.
protection for personnel does not eliminate the need for 11. R.P. Palluzi, Performance analysis of small size pilot plant
adequate pressure relief in all installations but can serve as and laboratory relief valves, Process Saf Prog 22 (2003),
an additional layer of protection against personnel injury. 137–140.

Process Safety Progress (Vol.32, No.1) Published on behalf of the AIChE DOI 10.1002/prs March 2013 27