Inherently Safer Design Concepts Applied to

Laboratories
Amy E. Theis and Charles F. Askonas
Fauske & Associates, LLC, Burr Ridge, IL 60527; theis@fauske.com (for correspondence)
Published online 23 April 2013 in Wiley Online Library (wileyonlinelibrary.com). DOI 10.1002/prs.11590

Several types of experiments are performed in laboratories

at Fauske & Associates, LLC (FAI). Test equipment includes
calorimeters to characterize reactive chemical systems and
multiple instruments to characterize both combustible dust
and gas/vapor explosions. It is a challenge to ensure that
each project is completed safely, since a variety of chemicals
are used and tested under extreme conditions. It is vital to
ensure the safety of people, property, and the environment at
all times. This requires first identifying the hazards (including rigorous review of material safety data sheets) and then
implementing adequate engineering and administrative
controls as necessary. This article will document best practices including management commitment, predicting and
eliminating hazards during extreme test conditions, and
implementing inherently safer design concepts to laboratory
C 2013 American Institute of Chemical Engineers Process
testing. V
Saf Prog 32: 142145, 2013

Keywords: laboratory safety; hazard identification; inherently safer design (ISD); MSDS Review.

MANAGEMENT COMMITMENT

It is essential that a safety culture is established and

emphasized by top-level management. It is FAI company
policy to employ a safety first principle for all jobs with no
exceptions. This directive is reinforced by the highest level
of management and is engrained in the company culture.
Management is committed to providing each employee with
the appropriate equipment and resources to maintain safe
working conditions. This safety directive is given by the President, reiterated by management, and communicated to all
employees at regular department meetings. Each employee
is given an opportunity to express workplace safety concerns
during these meetings or directly to their supervisor at any
time. This input is taken seriously by management, assigning
action items/due dates to responsible personnel in order to
address and resolve concerns. No job is performed without
understanding the safety concerns and ensuring that the
appropriate equipment and facilities are available.
HAZARD IDENTIFICATION AND ASSESSMENT

INTRODUCTION

The focus of this article will be to show experimenters

how to design and execute hazardous tests, such as calorimetry testing, flammability testing, and dust explosion testing.
The principles could be applied to any laboratory scale testing. Dust testing services typically involve performing the
same procedures on a variety of different chemicals. For this
type of testing, the material safety data sheet (MSDS) is the
most important safety document to review. Calorimetry testing and flammability testing involve customized test procedures on a variety of different chemicals. These tests
typically require a more thorough safety review.
As a laboratory that provides process safety information,
it is common to perform testing to understand the reactive
chemistry, and combustible characteristics of flammable dust
and vapors. A key component of laboratory safety is
predicting possible consequences (temperature, pressure,
corrosivity, and toxicity) based on test conditions for the
experiment. It is a misconceived notion that small-scale testing means small-scale hazards. This is not true and can lead
one to a false sense of security. Prior to each test campaign,
a hazard identification process must be conducted in order
to determine an appropriate hazard control strategy utilizing
inherently safer design concepts to ensure that personnel,
equipment, and property are adequately protected [10].

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The hazards of a chemical or intended chemistry must

first be identified. Several resources are available to identify
and assess hazards of chemicals [1,2] as well as hazards due
to chemical interactions [3]. The hazard identification process
begins with an MSDS review for each chemical that is to be
used for testing. It is recommended to obtain the MSDS from
the original manufacturer, since these tend to be most complete and provide the most detail. The following is a list of
tips to ensure thorough MSDS review.
MSDS Review Checklist
1.
2.
3.
4.
5.
6.

Volatility
Toxicity including health hazards and routes of entry
Corrosive properties
Reactivity with air, water or moisture
Unique properties
Verify safety information from more than one source. The
most conservative information should be used to develop
safe handling and test procedures
7. N/A means not available. Contact the technical support
of the manufacturer for more information
In some cases, the MSDS for a chemical does not provide
enough information for an appropriate safety review. This
can be due to many reasons. If the hazards identification section is brief or limited, a call to the technical support person
of the manufacturer is recommended in order to understand
the material better. The composition of the material with the
identification of the chemicals (and CAS numbers if
Process Safety Progress (Vol.32, No.2)

available) is important. Vague descriptions such as 90% solvent/inert, 10% reactive material do not provide enough information to determine the hazard of the material. A material
that is inert according to the manufacturer does not mean
that it could not decompose, react, or form a corrosive material when exposed to elevated temperatures. If the material
is a solvent, it must have a boiling point, density, and other
physical properties that need to be identified prior to testing.
For a material in development, test data may be limited or
not available. Contacting the chemist (or technical support
person) at the manufacturer is helpful, because they can
indicate generally whether it is acidic, basic, or neutral. In
some cases, testing may not have yet been performed on the
material, so they cannot provide specific ranges for flammable
limits, but some general information may be available. It is
not safe to assume that N/A means Not Applicable. It typically means Not Available and further investigation is necessary. If information cannot be obtained, the test is designed to
minimize or eliminate the hazard if it should be present.
Information regarding exposure controls are reviewed
and compared with information provided in the NIOSH
pocket guide [4]. If an MSDS for an exact chemical match
cannot be found, the MSDS for a chemical with the same
structure or functional groups can be used as a reference.
The most conservative values are used for the test design.
Personal protective equipment (PPE) required by the MSDS
are used at a minimum. In some cases, additional pieces of
PPE are selected for an increased level of protection.
The MSDS specifies the suitable fire extinguishing media
required for the chemical. This should be readily available in
the laboratory while tests are being performed. Proper PPE
should be worn in case of an accidental release or spill.
Appropriate clean-up equipment and procedures should be
readily available, and personnel should understand the procedures to follow if a spill should occur. For instance, when
strong acids are used, a bucket of water with baking soda or
caustic is readily available to neutralize a chemical spill.
Appropriate handling and storage conditions for the material should be followed. Information regarding storage, stability, reactivity, and proper disposal conditions is also
important. The MSDS should also indicate materials to avoid.
The chemical incompatibilities can be used to determine suitable materials for testing.
The National Fire Protection Association (NFPA) has
developed a system for indicating the health, flammability,
reactivity, and special hazards for many common chemicals
through use of the NFPA 704 Diamond. Ratings for health,
flammability, and reactivity range from 0 (no hazard) to 4
(most hazardous). These ratings apply only to the individual
chemicals, not to a mixture of chemicals. Additional information beyond the individual NFPA ratings is needed to identify
the hazards associated with the chemicals and test conditions
for a proposed experiment.
Another resource for chemical information is the Coast
Guard Chemical Hazards Response Information System
(CHRIS) [5], which provides chemical, physical, thermodynamic, toxicological, and fire properties for more than 1,000
chemicals. This information serves as an excellent supplement to the MSDS.
In addition to the MSDS, a chemical test questionnaire is
required for calorimetry testing. This contains critical information including the test recipe (composition), test conditions and procedure, chemical structures of reactants,
stoichiometry for the expected reaction, material incompatibilities, and possible decomposition products. Hazard identification of chemicals (reactants, intermediates, and products)
and the expected or possible chemistry/reactions is crucial to
developing an appropriate control strategy. The possible
decomposition products are important to understand,
Process Safety Progress (Vol.32, No.2)

Figure 1. U.S. DOT poison inhalation hazard zones for

liquids and gases. [Color figure can be viewed in the online
issue, which is available at wileyonlinelibrary.com.]

because these can be generated if high temperatures are

experienced during the test. By examining the functional
groups of the raw materials, possible decomposition products are predicted using organic chemistry reaction mechanisms [6]. Elevated temperatures during testing can lead to
elevated pressures that could then lead to unwanted decomposition or side reactions that should be anticipated before
testing is performed. Likely functional groups leading to
energetic decompositions should be given special attention
[7]. In these cases, the peak pressure is estimated for a specified amount of sample in a given reaction vessel to ensure
that it can be safely accommodated.
It is also necessary to determine the amount of chemical
to be handled or released, exposure limits (skin and inhalation) [4], U.S. Department of Transportation (DOT) hazard
class and Poison Inhalation Hazard (PIH) zone [8], flammable/explosion properties, and boiling point/vapor pressure
data (for gas or liquid).
The quantity of material handled or released directly
impacts the hazard associated with the process. For instance,
some tests require only a few grams of material while some
tests require several hundred grams. However, for highly
toxic materials, even a few grams of material may require
special handling procedures and high supervision or evacuation of the area to limit exposure to personnel. The quantity
of material affects the handling approaches and control
measures required for handling a chemical.
The DOT PIH zone is a useful index for determining the
toxicity of a material (see Figure 1) [8]. Classifications are A,
B, C or D with A being the highest and D being the lowest.
For gases, the PIH zone is a function of the inhalation toxicity. For liquids, the volatility (vapor concentration) and the
lethal concentration are factored into assigning the hazard
zone. Careful attention is given to test campaigns that utilize
chemicals in DOT hazard class 2.3 that are poisonous gases.
Learning from past experiments is invaluable. Providing
process safety data to industry for more than 25 years has
resulted in several thousands of experiments being performed in our laboratories. This experience can be used to

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predict or anticipate possible test conditions including

maximum temperature, pressure, material compatibility,
equipment problems, decomposition temperature, sample
behavior (tendency for foaming, etc.), and general lessons
learned. Any experience the client has performing tests with
this chemistry on the bench top is also useful. Adiabatic data
is more conservative than bench top data. It is typical for adiabatic experiments to yield higher temperatures and higher
pressures as well as higher rates of temperature and pressure
rise compared to bench scale testing.
In order to ensure that proper measures are taken to
safely perform testing and accommodate all decomposition
products, a detailed hazard review is performed on identified
hazards. Inherently safer design methodologies of minimization, substitution, moderation, and simplification are used to
manage or control the hazard. These are applied to both engineering controls and administrative controls (including
PPE).
Engineering controls are the first line of defense against
hazards. This includes proper ventilation to minimize personnel exposure to hazardous materials. NFPA 45 [9] can be
used for specific guidance on this and other design-related
issues. Ventilation can be accomplished using a laboratory
fume hood. For smaller quantities, a local ventilation vacuum
system can be used. Flammability testing should be performed in a concrete bunker, and equipment can be instrumented to operate remotely if it is necessary. Choosing a
location that can safely accommodate the anticipated hazards
for raw materials, intermediates, desired and decomposition
products from an experiment is important to maintain
employee and workplace safety. For highly toxic materials
(e.g., hydrogen cyanide), on-site testing is performed at a
customer facility.
Proper equipment selection is an example of an engineering control. Choosing a test cell material that is compatible
with the reactants, products, and potential decomposition
products is critical to maintaining safe working conditions,
reducing undesired side reactions, and ensuring successful
completion of the experiment. If a material is corrosive to
stainless steel, Hastelloy can be substituted to protect against
corrosion. The material of the vessel should also be able to
withstand the expected maximum pressure of a test or have
a relief path installed to safely relieve the accumulated
pressure.
If a sample is reactive with oxygen or air, the test cell will
be purged with nitrogen in order to reduce the initial oxygen
concentration in the system. An alternative would be to handle the material in a glove box with nitrogen atmosphere.
Performing an experiment with a smaller amount of sample is an example of minimizing the hazard. For instance, a
smaller size test apparatus such as the Advanced Reactive
System Screening Tool (ARSST, 10 mL of sample in 350-mL
containment) can be used instead of the Vent Sizing Package
(VSP2, 80 mL of sample in 4-L containment) for a toxic gassy
system where hydrogen sulfide could possibly be generated.
The ARSST has also been successfully used to minimize the
quantity of toxic raw materials such as hydrazine hydrate. If
a customer is not familiar with the chemistry, a screening test
[typically by Differential Scanning Calorimetry (DSC) using a
high-pressure crucible] can be performed to characterize the
material.
PPE is a key component to minimize personnel exposure
to a hazard. The required PPE depends on the quantity of
material being handled or generated. PPE includes eye/face
protection, hand/body protection, ear, and inhalation protection (respirators). Typically, the minimum requirement for
testing is safety glasses, lab coat, and nitrile gloves. After

review of the MSDS, additional protection such as goggles

(for acids or bases), face shield, TyvekV suit (for strong skin
irritants), half or full face respirator, or other PPE may be
deemed necessary. In cases where filtering cartridges are not
effective, a supplied air respirator is used. The supervisor
reviews the required PPE with the test personnel prior to the
experiment to ensure they are comfortable wearing and
properly using the equipment as well as understanding the
hazard posed by the chemical(s). In cases where PPE is burden-some to wear (e.g., self-contained breathing apparatus),
the required amount of time to wear the equipment is minimized (if possible). In some cases, two people are assigned
to a particular task to create a buddy system.
For highly toxic materials (chlorine gas or ethylene oxide), the quantities of raw materials are limited to only the
necessary amount. This can mean ordering the minimum
amount of material to be used for testing. Another strategy
would be to meter in a raw material instead of performing a
batch addition, to minimize the material contact and therefore heat or pressure generation. Another protective strategy
for highly toxic chemicals includes procedural controls to
minimize personnel exposure. Handling guidelines and
restrictions have been developed that define safe handling
and disposal procedures for these types of chemicals.
Substitution is another inherently safer concept that can
be applied for the safe handling of chemicals in the
laboratory. Typically, the chemistry to be performed is not
flexible. However, it is possible to substitute a different
chemical for cleaning. One example is using baking soda
and water solution for cleaning instead of caustic. For
strongly acidic chemicals, caustic is necessary and appropriate. If the potential acidic product is mild, then baking soda
and water is sufficient. The hazard control measure should
be proportional to the identified hazard.
Another consideration for inherently safer handling a
chemical is moderating the effect of a material. One way to
accomplish this is to use a dilute solution instead of a stronger one. Neutralization procedures are implemented when
poisonous gases are suspected to be formed, which limits
personnel exposure, minimizes the quantity, and reduces the
toxicity of the released material.
For a reaction that is expected to generate a
noncondensable gas, the headspace volume of the test may
be increased in order to moderate the pressure rise rate. This
could be accomplished by performing an ARSST experiment
instead of a VSP2 experiment as previously mentioned or by
performing an open system VSP2 test (4-L headspace) instead
of a closed VSP2 test (0.040-L headspace). The expected pressure of a test is calculated based on any expected pressure
generation as well as the vapor pressure of the mixture given
the expected temperature range of the experiment. This information is used to determine the proper selection of containment/test vessel, required pressure of nitrogen supply, and
emergency test shut down procedures, if necessary.
Controlling the hazard can utilize the inherent safer concept of simplification. One example is to reduce the number
of fittings in the test apparatus to minimize the potential for
leaks. Other considerations for simplification include the test
equipment as well as handling and disposal of the chemical.
Efforts are made to handle chemicals as close to room temperature as possible. Some tests require subambient or elevated temperatures. In these cases, administrative controls
(procedures) and PPE are used to ensure personnel safety.
An active engineering control is to specify shut down criteria in the software program. This would be for situations
where the outcome is well understood. Some equipment or
experiments may require additional supervision if the chemistry is not well defined or if consequences due to a deviation in the operations could be highly hazardous.

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Appropriate control strategies are identified in test procedures that serve as administrative controls. Other administrative controls include safe handling procedures for unique
chemicals such as compressed or corrosive liquids and acid
gases.
CONCLUSIONS

Test personnel should be prepared to safely accommodate and dispose of all foreseeable reaction and decomposition products. Identifying the hazards given the reactants,
test conditions, and expected desired and potential decomposition products is critical. The required test equipment,
PPE, and test procedures must be identified to perform the
test, disassemble the apparatus, and dispose of all materials
safely. In summary, the components for maintaining a safe
work environment include: a safety culture established and
valued by management, diligent hazard identification, and
developing a hazard control strategy utilizing inherently safer
design concepts.

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