Testing Methods
[Link] Assessment and Testing Strategies
Information on understanding the hazards depends on the stage of development of the
process as indicated in Table 3.4. During early developmental chemistry work, only
small amounts of materials will be available. In many cases, only theoretical information
from the literature or from calculations is readily available.
Table 3.4 Suggested Stages in Assessment of Reactivity by Scale
Stages
1. Development Chemistry-Characterization of
materials
2. Pilot Plant - Chemical reaction hazards
3. Full-Scale Production - Reevaluation of chemical
reaction hazards
Aspect
Characterization of process alternatives
Choice of process
Suitability of process
Screening for chemical reaction hazards
Influence of plant technology regarding potential
hazards
Definition of safe procedures
Effects of expected variations in process conditions
Definition of critical limits
Newly revealed reactivity hazards from plant
operations
Management of changes
Update of safety procedures as required
Ongoing hazard assessment in examining potential
deviations from process conditions through
interaction of process safety with engineering and
production, personnel
Screening tests can be run to identify reaction hazards. Also, data for pilot plant
considerations should be evaluated and obtained as necessary. In the pilot plant stage,
additional material becomes available so that the reaction hazards can be investigated
more extensively. Process control features and deviations from normal operating
conditions should be checked. Operating procedures can be drafted and checked.
Emergency procedures can be defined.
3. BASIC PHYSICAL PROPERTIES / THERMAL STABILITY DATA 57
During full-scale production, particularly initially, chemical reaction hazards may be
reevaluated. More tests may be necessary as a consequence of increased knowledge of
the process, changed production requirements, or other process changes such as the use
of different feedstocks.
A typical chronology for testing is shown in Table 3.5. The tests provide either
qualitative or quantitative data on onset temperature, reaction enthalpy, instantaneous
heat production as a function of temperature, maximum temperature, and / or pressure
excursions as a consequence of a runaway reaction. The choice of test equipment to be
used depends on the conditions, such as scale, temperature, mixing, and materials of
construction, at which the substance or mixture is to be handled. The interpretation of
the data from each of these tests is strongly dependent on the manner in which the test is
run and on the inherent characteristics of the testing device. Guidance is provided along
with each test description, particularly in the detailed sections later in this chapter.
Table 3.5 Typical Testing Procedures by Chronology
Subject
Identification of exothermic activity
Explosibiiity of Individual
substances
Compatibility
Normal reaction
Minimum exothermic runaway
temperature
Consequence of runaway reaction
Property to Be Investigated
Thermal Stability
Detonation
Deflagration
Reaction with common
contaminants (e.g., water)
Reaction profile
Effect of change
Gas evolution
Establish minimum temperature
Temperature rise rates
Gas evolution rates
Typical Instrument Information
DSC/DTA
Chemical structure
Tube test
Card gap
Drop weight
Oxygen balance
High rate test
Explosibiiity tests
Specialized tests
Bench-scale reactors (e.g., RC1)
Adiabatic Dewar
Adiabatic calorimetry
ARC
Adiabatic Dewar
Adiabatic calorimetry
ARC
VSP/RSST
RC1 pressure vessel
ARC = Accelerating Rate Calorimeter
DSC = Differential Scanning Calorimeter
DTA = Differential Thermal Analysis
RC1 = Reactor Calorimeter
RSST= Reactive System Screening Tool (Ref. 3-31)
VSP = Vent Size Package
58 GUIDELINES FOR ENGINEERING DESIGN FOR PROCESS SAFETY
Experimental hazard evaluation includes thermal stability testing, solid flammability
screening tests, explosibility testing, detailed thermal stability and runaway testing, and
reactivity testing.
The recommended experimental evaluation is condensed in a number of flowcharts
which, in general, follow the most reliable and internationally recognized standard test
methods. Details of the strategic testing scheme are covered in the following section.
