UNIT 2 – COMPUTER AIDED INSTRUMENTS

Thermal Analysis / Calorimetry:

Thermal analysis and calorimetry are ways to measure temperature changes and a
material's reaction to those changes. Thermal analysis is a method used to measure
properties of a material at different temperatures. Many characteristics of a sample can be
measured as a function of temperature, including volume, mass, dimension, optical
properties, gaseous decomposition products, heat difference, and temperature difference.
To perform thermal analysis, both the temperature and sample environment are controlled.
The temperature is steadily increased or decreased and tests are done at a series of
temperature points to see if or how a material is changing.

Calorimetry is used to measure the heat released into or absorbed from the environment
during a chemical reaction. There are three main classes of calorimeters: isothermal, which
uses a heat sink to keep the reaction environment at a constant temperature as the reaction
occurs; adiabatic, which allows reactions to change the environment and the change in
temperature is measured as time goes on; and temperature scanning, in which the
difference in the amount of heat required to increase the temperature of the sample being
tested and a reference sample is determined.
Applications:
Thermal analysis and calorimetry are used in electronics industries to help determine and
maintain stability, safety, and quality control of their products. Other applications include:
 Materials science
 Pharmaceutical
 Food analysis
 Energy
 Analytical Chemistry
 and more
Differential Scanning Calorimetry (DSC)
DSC is the generic term for the following two measurement methods.
 Heat Flux DSCs
A technique in which the temperature of the sample unit, formed by a sample and
reference material, is varied in a specified program, and the temperature difference
between the sample and the reference material is measured as a function of
temperature.
 Power Compensation DSC
A technique in which difference of thermal energy that is applied to the sample and
the reference material per unit of time is measured as a function of the temperature
to equalize their temperature, while temperature of the sample unit, formed by the
sample and reference material, is varied in a specified program.
Description of DSC

Figure 1. Block diagram of Heat Flux DSC

DSC is a commercially available instrument which has two (2) types: Heat Flux Type
and Power Compensation Type. Figure 1 shows the block diagram of Heat Flux DSC as an
example. Heat Flux DSC comprises the sample and reference holder, the heat resistor, the
heat sink, and the heater. Heat of heater is supplied into the sample and the reference
through heat sink and heat resistor. Heat flow is proportional to the heat difference of heat
sink and holders. Heat sink has the enough heat capacity compared to the sample. In case
the sample occurs endothermic or exothermic phenomena such as transition and reaction,
this endothermic or exothermic phenomena is compensated by heat sink. Thus the
temperature difference between the sample and the reference is kept constant. The
difference the amount of heat supplied to the sample and the reference is proportional to
the temperature difference of both holders. By calibrating the standard material, the
unknown sample quantitative measurement is achievable.
DSC enables the measurements of the transition such as the glass transition, melting,
and crystallization. Furthermore, the chemical reaction such as thermal curing, heat history,
specific heat capacity, and purity analysis are also measurable. Recently, with the
development of the highly-functional polymeric material, these thermal properties analysis
needs are increasing dramatically. DTA and DSC detect the temperature differences
between the sample and the reference; however, DSC can perform the quantitative
measurement of the amount of heat on top.
Thermogravimetric analysis:
Thermogravimetric (TG) is a branch of thermal analysis examining the mass changes
of a sample as a function off temperature (in the scanning mode) or as a function of time (in
the isothermal mode).
Thermal gravimetric analysis or thermogravimetric analysis (TGA) is a method of
thermal analysis in which changes in physical and chemical properties of materials are
measured as a function of increasing temperature (with constant heating rate), or as a
function of time (with constant temperature and/or constant mass loss).
• Changes in the mass of a sample due to various thermal events (desorption, absorption,
sublimation, vaporization, oxidation, reduction and decomposition) are studied while the
sample is subjected to a program of change in temperature. Therefore, it is used in the
analysis of volatile products, gaseous products lost during the reaction in thermoplastics,
thermosets, elastomers, composites, films, fibers, coatings, paints, etc.
• There are different types of TGA available:
i. Isothermal or Static TGA: In this case, sample is maintained at a constant temperature for
a period of time during which change in weight is recorded.
ii. Quasi-static TGA: In this technique, the sample is heated to a constant weight at each of a
series of increasing temperature.
iii. Dynamic TGA: In this type of analysis, the sample is subjected to condition of a
continuous increase in temperature at a constant heating rate, i.e., usually linear with time.

• The instrument used for TGA analysis is a programmed precision balance for a rise
in temperature (called as Thermobalance, see Figure 23.01). Thermobalance
consists of an electronic microbalance (important component), a furnace, a
temperature programmer and a recorder.

Figure 23.01: Block Diagram of a Thermobalance.

• The plot of mass change in percentage versus temperature or time (known as TGA
curves) is the typical result of TGA analysis as shown in Figure 23.02.

Figure 23.02: The plot of mass change with temperature.

• There are two temperatures in the reaction: Ti (starting of decomposition

temperature) and Tf(final temperature) representing the lowest temperature at
which the onset of a mass change is seen and the lowest temperature at which the
process has been completed, respectively. The reaction temperature and interval
(Tf - Ti) strongly depend on the conditions of the experiments. Hence, they can not
have any fixed values.

Applications of TGA:

a) Thermal stability of the related materials can be compared at elevated

temperatures under the required atmosphere. TGA curve helps to explicate
decomposition mechanisms.
b) Materials Characterization: TGA curves can be used to fingerprint materials for
identification or qualitycontrol.
c) Compositional analysis: By a careful choice of temperature programming and
gaseous environment, many complex materials/ mixtures can be analyzed by
decomposing or removing their components. For example: filler content in polymers;
carbon black in oils; ash and carbon in coals, and the moisture content of many
substances.
d) Kinetic studies: A variety of methods can be used to analyze the kinetic features
of weight loss or gain through controlling the chemistry or predictive studies.
e) Corrosion studies: TGA provides a means of studying oxidation or some reactions
with other reactive gases or vapors.
Accelerating Rate Calorimeter

Purpose
The ARC is used to characterize the reactive nature of a chemicals. The substance is place in
the small container (35 ml) shown below and then installed in the apparatus (also shown
below). The ARC has two heating modes: (1) heat and search, and (2) heat.

In the heat and search mode, the substance is heated by fixed temperature increments, say 5
deg. C., and then the ARC waits at the specified temperature until an exotherm is detected. If
an exotherm is detected, the ARC goes into adiabatic mode and follows the exotherm. If an
exotherm is not detected, then the ARC moves to the next higher temperature.

In the heat mode, the temperature is increased continuously until an exotherm is detected, at
which point the ARC goes into adiabatic mode and follows the exotherm.

Data

The data from the ARC test includes the temperature and pressure as a function of time.
These data can be used to calculate the following parameters used to characterize reactive
chemicals:
 maximum self-heat rate
 maximum pressure rate
 onset temperature
 reaction order and Arrhenius parameters
 others as required

Sensitivity

The ARC is capable of detecting self-heat rates as low as 0.01 deg. C per minute and as high
as 10 deg. C per minute. The major problem with the ARC is the high thermal inertia of the
reactor vessel, which may produce misleading results under some conditions.

These are the ARC bombs. The bomb on the

right has been sawed open to show the insides
and wall thickness. Bombs are available in a
variety of materials. Bombs are available that
can withstand pressures as high as 35,000 psi.
A thermocouple clips on to the outside of the
bomb to measure the temperature.
This shows the inside
of the containment
vessel. The bombs are
heated by an upper
and lower heater. The
bomb is located at the
colored spot.

This is a close-up view of

the heaters and the location
of the bomb. Notice the
thermocouple clipped on to
the side of the bomb. The
pressure transducer is also
shown.

Reaction calorimeter:

A reaction calorimeter is a calorimeter that measures the amount of energy

released (exothermic) or absorbed (endothermic) by a chemical reaction. These
measurements provide a more accurate picture of such reactions.

Reaction calorimeters – how do they work?

It is possible to split reaction calorimeters into four groups, depending on the

measurement technique used:

1. Heat flow calorimeters (HFC)

The first specialized reaction calorimeter was designed around the principle of
heat flow, and it is still considered an industry standard to this day. The
measurement vessel is essentially a jacketed reactor, and signals from temperature
probes are used to calculate heat flux through the reactor wall, using the following
equation (under steady-state conditions):
 Where: Q is rate of heat transfer [W]; U is overall heat transfer coefficient [W
(m2 K)-1]; A is heat transfer area [m2]; Tr is process temperature; Tj is reactor jacket
temperature.

This technique has one major disadvantage. Since the U and A can change
during the experiment, it is necessary to perform calibration to determine the UA
before and after the experiment. When UA is known, the data is processed using the
values obtained to correct it. The UA is determined by using a calibration heater of
known power.

This means this method has limited use when UA changes considerably
(change in viscosity, density, reactor fill volume). Those changes are often non-
linear, and they are very challenging to correct (torque measurements etc.). Such
corrections are normally sufficient for safety studies, however, heat flow calorimeters
struggle when big changes of UA are observed. Because of the calibration pulses,
the method can’t provide real-time data (as they are corrected afterward using the
UA obtained from calibration).

The typical workflow of the Isothermal heat flow calorimeter is the following:

1. Reach desired reaction temperature using circulator and reaching steady

state conditions
2. Perform pre-calibration pulse using a calibration heater to determine initial UA
value
3. Afterward, the reaction takes place with desired process conditions (additions
etc.)
4. Post-calibration pulse to determine final UA value
5. Data processing, interpolating the UA values (done automatically), and
calculating the specific enthalpy of the reaction (kJ), and calculating the
scalable value (kJ mol-1).

2. Power compensated calorimeters

Power compensated calorimetry (PCC) is the other widespread method of
performing reaction calorimetry – it is a variation of heat flow calorimetry (HFC). The
measurement of power is determined by the following simplified equation (under
steady-state conditions):

Where: Q is the rate of heat transfer [W]; I is the current supplied to heater
[A]; I0 is the current supplied to the heater at steady conditions before experiment
[A], U is the voltage supplied to the heater [V].
 The system uses a cooling jacket with constant flow and temperature of the
coolant, which is typically set 5 – 20 °C below desired process temperature. The
process temperature is then maintained by the electrical heater with a large surface
area. As the heat load of the reaction changes, the power of the heater is controlled
to maintain isothermal conditions – so the inverse power supplied to the heater
equals the heat generated / absorbed by the reacting system in the vessel.

The major advantage of this method is that it doesn’t require calibration, as

the heater of known power is used to control the temperature of the reaction, shows
real-time data, and typically, the system can achieve a faster thermal response,
since electrical-based heating will respond faster than an oil-based system.

The major (experiment-dependent) disadvantage of power compensation

calorimetry is the creation of hotspots created by the heater; these result in
temperature gradients around the heater which can lead to local initiation of
reactions. Power compensation calorimetry is also sensitive to changes in UA (as is
heat flow calorimetry), and the maximum exotherm is limited by the available power
of the heater.

Typical workflow of a power compensation calorimetry experiment (where the UA

change is not considered):

1. Heating: Reach the desired temperature with the heater (constant high power)
and circulator on
2. Settling: Once the desired temperature is reached, the heater remains on
constant power and the circulator controls the temperature to reach steady
state conditions
3. Zeroing: Circulator temperature is fixed, and heater power is varied to keep
the reactor at the desired temperature
4. Reaction takes place with desired process conditions (additions etc.), while
the exotherm is controlled by varying the power of the heater. The inverse
value of the heater power shows actual reaction power
5. Data processing

3. Heat balance calorimetry

Heat balance calorimetry is slightly different, as it uses data obtained from

jacket flow for calculation of the heat release / absorption. The difference between
coolant temperature entering and leaving jacket is used to calculate heat exchange.
The heat generated / absorbed by the system under steady-state conditions is as
follows:
 Where: Q is rate of heat transfer [W]; mc is mass flow of the coolant [kg s -1];
Cp si specific heat capacity of the coolant at given temperature [J (kg K) -1] , Toutlet is
outlet temperature of coolant [K], T inlet is inlet temperature of coolant [K], Q losses are
thermal losses to the environment [W].

This method isn’t very often used in reaction calorimetry, but is very valuable
in accessories, as this principle is used with reflux condensers used in reaction
calorimetry, to calculate the cooling power of the condenser. However, it usually
requires higher exotherms (to create the temperature gradient between jacket
inlet/outlet) and is very sensitive to heat loss to the environment, which can be
challenging to determine. However, compared to PCC and HFC it is not generally
affected by changes in UA.

4. True heat flow calorimetry

True heat flow principle can be considered as a 2 nd generation reaction

calorimetry principle, as it removes most of the shortcomings of the methods
described above. The main difference between true heat flow calorimetry and other
forms of reaction calorimetry is a different reactor vessel construction, that doesn’t
use oil as means of temperature control. It is a unique solution, that is used
exclusively by Chemisens CPA 200 series calorimeters.

The main difference in the reactor is that the temperature control is achieved
by use of Peltier element, which controls the temperature in the reactor via its metal
base. The metal base contains a heat flow transducer, and since it is the only and
well-defined area where heat transfer between reactor contents and the environment
is achieved, it is not very susceptible to changes in UA.

The heat measured using this principle follows this equation:

Where Q is the rate of heat transfer [W]; λ is the heat flow transducer heat
conductivity [W (m K)-1]; A is heat flow transducer area [m 2] and dT/dX is the
measured temperature gradient over the transducer disk [K m-1].

From the equation, it is visible that none of the parameters are dependent on
reactor contents, and don’t change during the experiment; this eliminates many
shortcomings of the methods above and introduces advantages over them. For an
additional level of precision, the whole reactor is placed inside in liquid bath with
precise temperature control, which is kept at the same temperature as the reactor.

A major advantage of true heat flow calorimetry is that the reactor doesn’t
require routine calibration; the reactor is calibrated during the manufacturing
process.
 A major benefit of true heat flow calorimetry for the user is that that the
baseline doesn’t change over the course of the experiment (as with other methods
due to changes in UA), so it’s not affected by changes in viscosity, fill volume, etc.,
and it delivers a higher level of accuracy and sensitivity (resolution down to 0.0001W
for the Chemisens HighSens Calorimeter).

REACTIVE SYSTEM SCREENING TOOL (RSST)

The RSST (Figures 1 and 2) consists of a spherical glass reaction vessel and
immersion heater (optional), its surrounding jacket heater and insulation,
thermocouples and a pressure transducer, a stainless steel containment vessel that
serves as both a pressure simulator and safety vessel, and, not shown, a magnetic
stirrer base, a control box containing the heater power supply, temperature
amplifiers, and a data acquisition and control panel. The sample cell volume is 10 ml
and the containment volume is 350 ml. A key feature of the apparatus is its low
effective heat capacity relative to that of the sample whose value, expressed as the
capacity ratio, is approximately 1.04 (i.e., quite adiabatic). This feature allows the
measured data to be directly applied to process scale.

Typically, a 10 mλ sample is heated at a constant rate and the sample self-

heat rate is found as a function of sample temperature. The imposed linear ramp rate
can be varied from 0.1ºC/min. to ramp rates approaching those required to simulate
fire exposure by using the immersion heater option. The heater compensates for
losses, and the self-heating rate of an exothermic system is adjusted for heater
input. Reagents may be added to a sample during a test. Data handling programs
produce plots of pressure vs. temperature, temperature vs. time, pressure vs. time,
and Arrhenius plots.

The RSST quickly and safely determines the potential for runaway reactions
and measures the rates of temperature and, in case of gassy reactions, pressure
increases to allow reliable determinations of the energy and gas release rates. A
recent additional feature of the RSST allows flow regime characterization, i.e.,
"foamy" versus "non-foamy" behavior, to be determined under actual runaway
conditions (Fauske, 1998). This information can be combined with analytical tools
(summarized later) to assess reactor vent size requirements.

EXPLOSIVE TESTING:

The safety testing of explosives involves the determination of various

properties of the different energetic materials that are used in commercial, mining,
and military applications. It is highly desirable to measure the conditions under which
explosives can be set off for several reasons, including: safety in handling, safety in
storage, and safety in use.

It would be very difficult to provide an absolute scale for sensitivity with

respect to the different properties of explosives. Therefore, it is generally required
that one or more compounds be considered a standard for comparison to those
compounds being tested. For example, PETN is considered to be a primary
explosive by some individuals, and a secondary explosive by others. As a general
rule, PETN is considered to be either a relatively insensitive primary explosive, or
one of the most sensitive secondary explosives. PETN may be detonated by striking
with a hammer on a hard steel surface (a very dangerous thing to do), and is
generally considered the least sensitive explosive with which this may be done. For
these facts and other reasons, PETN is considered one standard by which other
explosives are gauged.

Another explosive that is used as a calibration standard is TNT, which was

afforded the arbitrary Figure of Insensitivity of 100. Other explosives could then be
compared against this standard.

Types of safety testing:

 Impact testing. The impact testing of explosives is performed by dropping a

fixed weight onto a prepared sample of the explosive to be tested from a
given distance. The weight is released, impacts upon the sample, and the
result is noted. The impact distances are determined and the results are
analyzed by the sensitivity test and analysis methods selected. The two most
common sensitivity test and analysis methods are the Bruceton
analysis and Neyer d-optimal test. These methods allow the user to determine
the 50% initiation level (the distance at which 50% of the samples will "go"),
and a standard deviation. Impact testing may also be performed with liquid
samples confined in special cells.
 Friction testing. There are several techniques through which explosives may
be tested to determine their sensitivity to friction. One of the most popular is
the ABL friction test, which uses a line of explosives on a prepared metal
plate, placed in front of a specially prepared metal wheel that is forced down
upon the plate with a hydraulic press. The metal plate is then struck with a
pendulum to move it, squeezing the explosives between plate and wheel as
the plate moves. Initiation is determined, and analyzed by the Bruceton
analysis or Neyer d-optimal test, as above. BAM friction testing is similar,
 except that the sample is placed on a ceramic plate which is then moved side-
to-side as a ceramic peg exerts force on the sample.
 Electrostatic discharge. Testing for ESD, or "spark" sensitivity of explosives
is performed with a machine designed to discharge from a capacitor through a
prepared sample. The Sandia National Labs design employs a dipping needle
that punctures a sample cell and discharges the spark simultaneously. The
amount of energy discharged into the cell becomes the variable in
which Bruceton analysis or Neyer d-optimal test is performed to determine
spark sensitivity.
 Thermal sensitivity. Determining the point at which a compound is capable
of detonating under confinement with thermal stress is useful. A fixed quantity
of material is placed in an aluminum blasting cap shell, and pressed into place
with an aluminum plug. The sample is immersed in a hot metal bath, and the
time-to-detonation is measured. If over 60 seconds, a fresh sample is run
again at a higher temperature. In this manner, it is possible to determine the
temperature at which an explosive will detonate on the small scale. Unlike the
other tests above, this figure is misleading as explosives have more thermal
issues on the large scale. Therefore, the thermal sensitivity figures
established using this technique are higher than one would expect in the real
world. Thermal safety testing may also be performed via differential scanning
calorimetry, in which a small (sub-milligram) sample is placed in a sample cell,
and the temperature is increased slowly. The calorimeter determines how
much energy is required to increase the temperature of the sample. Using this
device, characteristics such as the melting point, phase transitions and
decomposition temperature of an explosive may be determined.

Deflagration Test:

Combustion (burning) is a process by which energy is released.

Deflagration and detonation are two ways energy may be released. If
the process propagates outward at subsonic speeds (slower than the speed
of sound), it's a deflagration. If the explosion moves outward at supersonic
speeds (faster than the speed of sound), it's detonation.

While the action of deflagration is to push the air in front it, objects do
not explode because the rate of combustion is relatively slow. Because the
action of detonation is so rapid, however, detonations result in shattering or
pulverizing objects in their path.

Deflagration:

The definition of deflagration, according to the Collins Dictionary is "a fire in

which a flame travels rapidly, but at subsonic speed, through a
gas. Deflagration is an explosion in which the speed of burning is lower than
the speed of sound in the surroundings."

Everyday fire and most controlled explosions are examples of deflagration.

The flame propagation velocity is less than 100 meters per second (usually
much lower), and the overpressure is less than 0.5 bar. Because it is
 controllable, deflagration can be harnessed to do work. Examples of
deflagrations include:

 internal combustion engine (used in any vehicle that uses fossil fuels such
as gasoline, oil, or diesel fuel)
 gas stove (fueled with natural gas)
 fireworks and other pyrotechnics
 gunpowder in a firearm

Deflagration burns outward radially and requires fuel to spread. Thus, for
example, a wildfire starts with a single spark and then expands in a circular
pattern if there is fuel available. If there is no fuel, the fire simply burns out.
The speed at which deflagration moves depends upon the quality of the
available fuel.

Detonation test:

The word "detonation" means "to thunder down," or explode. When a

decomposition reaction or combination reaction releases a lot of energy in a
very short span of time, an explosion may occur. A detonation is a dramatic,
often destructive form of an explosion. It is characterized by a supersonic
exothermic front (in excess of 100 m/s up to 2000 m/s) and significant
overpressure (up to 20 bars). The front drives a shockwave ahead of it.

Although technically a form of oxidation reaction, a detonation doesn't

require combination with oxygen. Unstable molecules release considerable
energy when they split and recombine into new forms. Examples of chemicals
that produce detonations include any high explosives, such as:

 TNT (trinitrotoluene)
 nitroglycerine
 dynamite
 picric acid
 C4

Detonations, of course, can be used in explosive weapons such as nuclear

bombs. They are also (in a much more controlled manner) in mining, road
construction, and the destruction of buildings or structures.

Minimum ignition energy:

The minimum ignition energy (MIE) of a dust cloud is the lowest energy
value of a high-voltage capacitor discharge required to ignite the most readily
ignitable dust/air mixture at atmospheric pressure and room temperature. The
dust concentration and the ignition delay are systematically varied until a
minimum value of the ignition energy is found. The tested energy levels are
1000, 300, 100, 30, 10, 3 en 1 mJ.

Importance
 It is well known that explosible dust clouds can be ignited by electric
sparks and arcs that occur in switches and motors, and in short-circuiting
caused by damaged cables. In addition, some categories of electrostatic
discharges may initiate dust explosions in industry.
For an assessment of the hazard situation in dust-processing installations,
knowledge of the minimum ignition energy is indispensable. This value can
possibly determine the extent and hence the cost of protective measures.

Test equipment & procedure

A modified Hartmann-tube made of glass with a volume of 1.2 litre is used as

the explosion vessel. The dust dispersion system at the base of the tube is of
the "mushroom-shaped" type around which the sample is loosely scattered. A
blast of compressed air at 7 bar is used to disperse the dust in the glass
cylinder where it is ignited by a spark between two electrodes.

The energy just sufficient to ignite the dust under investigation is

determined. This ignition energy is then successively reduced with variation of
the dust concentration and the ignition delay time (turbulence) in a series of
tests until no ignition takes place in at least 10 successive experiments. The
minimum ignition energy (MIE) lies between the lowest energy value (E2) at
which ignition occurred and the energy (E1) at which in at least 10 successive
experiments no ignition was observed. The energy range thus determined is
called the minimum ignition energy of a combustible dust in admixture with air.
However, for purposes of simplification often only the lower limit value (E1) is
specified as the minimum ignition energy (MIE): E1 < MIE < E2.

By definition, MIE data refer to protracted capacitor discharges. These

are generally more incendive than purely capacitive discharges. The results
obtained under such conditions (with inductance) can be applied to
operational conditions only if the capacitors occuring in plant installations ara
also discharged via an inductance. Hence, if the incendivity of electrical
discharges - especially of electrostatic discharges - with regard to dust/air
mixtures is to be assessed, the minimum ignition energy must also be
determined without an inductance in the discharge circuit. Therefore tests can
be performed both with an inductance (of 1 mH) as without inductance.
The test is performed on the sample fraction having a particle size less than
63 µm.

Friction Sensitivity

Friction is another stimulus for detonation of an explosive. The heat

generated due to the friction between explosive particles or explosive-working
surface can cause the detonation. The pendulum friction device developed by
the Bureau of Mines consists of a steel swinging shoe which is the bob of a
pendulum. The apparatus is shown in Fig. 1.25. The friction between the shoe
and anvil is controlled by controlling the number of swings of the pendulum. A
specially designed anvil is used in the test. At the central portion of the anvil
three parallel grooves are cut to prevent the test sample from being brushed
off from the surface by swinging shoe.
 During the test, the test explosive charge is spread on the anvil
surface. A steel shoe or one faced with red-hair fiber (called the “hard-fiber-
faced shoe”) is used. A trigger is used to allow the shoe to be dropped upon
the anvil from any desired vertical height ranging from 50 to 200 cm. The
normal height of drop used is 100 cm. This test should be conducted in a
temperature controlled room so that the temperature of the anvil and shoe is
70 ± 5 F. About 7 g of sample is spread evenly in and around the three
grooves on the anvil plate. The apparatus is adjusted with loaded weights to
provide about 18 ± 1 swings across the face of the anvil before coming to rest.
The shoe is then released and the test result is noted.

Twenty trials should be conducted using the steel shoe or fiber shoe.
The test material using the steel shoe should not react in any of the twenty
trials. Other friction sensitivity tests that are most common include ABL
Friction test (recommended by UN) and BAM friction test (recommended by
both US DOD and UN).

BAM Friction Test

In this method, the friction is generated between two porcelain objects

as shown in Fig. 1.27. A rough porcelain plate holds the sample that is moved
electro-mechanically against a stationary porcelain pistil. A force normal to the
plate is applied through the pistil and can be changed. The normal force at
which 50% of initiations occur is used as the measure of the friction
sensitivity. Generally the sample is tested as received.

For some explosives, a wetting agent is added for safe handling and
transportation. This type of sample is tested with the minimum content of
wetting agent. About 10 mg of the test sample is placed on the plate. The
stationary porcelain cylinder is lowered to the top the sample by using the
loading arm. A selected weight [mass] is attached to the arm to apply the
force, which may vary from 4.9 to 353.2 N. The movement of the plate, or the
stroke length, is 10 mm forward and backward from the initial position. The
occurrence of the initiation due to friction is determined from crackling sound,
appearance of smoke, or by the characteristic burning smell. Although both
methods can be used in evaluating safety in transport, in other hazard
assessments only the BAM test is specified (Fig. 1.28).
Gap Tests-Shock Wave:

The gap test is conducted to obtain the minimum shock wave pressure that
can cause complete detonation of the explosive. The design of the experimental
system depends on the size of the booster and the sample and is called either Small
Scale Gap Test or Large Scale Gap Test system. The choice of the small or large
scale gap test facility depends on the pressure and duration of positive phase of
pressure of the generated shock wave. The determine the sensitivity to the shock
wave, the complete detonation of the explosive charge must occur, which is
generally indicated by the formation a clean hole in the steel witness plate that is
9.53 mm thick. A small scale gap test system is shown in Fig. 1.30.