Introduction to Combustible

Dust Test Methods

Presented by:

Ashok Ghose Dastidar, PhD MBA,

Vice President, Dust & Flammability Testing and Consulting Services

16W070 83rd Street • Burr Ridge, Illinois 60527

(877) Fauske1 or (630) 323-8750 • Fax: (630) 986-5481 • E-mail: [email protected]
Presentation Agenda

 Introduction
 Combustible And Deflagrable Dust Testing Strategy
 STAGE 1: Material Identification
 STAGE 2: Sample Identification and Characterization
 STAGE 3a: Reactive as a Cloud (Deflagration)
 STAGE 3b: Reactive as a Pile or Layer (Combustion)
 STAGE 4a: Deflagration Testing
 STAGE 4b: Combustion Testing
 Questions and answers

2
Introduction

 Combustible dusts and powders are a serious hazard in the

process industries and behave differently than flammable
gases.
 Chemical composition affects its reactivity
• particle size distribution,
• particle morphology and
• moisture content.
 Increases the difficulty in generating test data.
 Many tests that can be performed to generate data that can
be used for the development of mitigation and prevention
strategies.
• Lead to some confusion as to which tests are necessary and when to
perform them

3
Combustible And Deflagrable
Dust Testing Strategy.

Stage 1
Material Identification

Stage 2
Sample Identification and Characterization

Stage 3a
Stage 3b
Reactive as a Cloud
Reactive as a Pile or Layer
(Deflagration)
(Combustion)
•Go/No Go Explosibility Screening
•Burning Behavior
•Burn Rate Screening

Stage 4a Stage 4b
Deflagration Testing Combustion Testing
•Explosion Severity (Pmax & KSt) •Burn Rate Test
•Minimum Explosible Concentration (MEC) •Layer Ignition Temperature (LIT)
•Minimum Ignition Energy (MIE) •Auto Ignition Screening (Grewer)
•Minimum Autoignition Temperature of a •Hot Storage Screening
Dust Cloud (MIT) •Exothermic Decomposition Screening
•Limiting Oxygen Concentration (LOC) •Smoldering Gas Evolution (Lütolf)

4
 STAGE 1:
Material Identification
Material Identification

 Establish exactly what chemical will be involved!

 What will be the “fuel” for combustion?
• Organic material
• Metals in particulate form can also burn!
 Look at all the particulate material that is composed of
organic material and metals.
 If an unknown material is present in the process either as a
byproduct or as a contaminant then further study is required.
 The NFPA standards as well as online databases have
examples of materials that have a potential for combustibility
or deflagrability.
 STAGE 2:
Sample Identification and
Characterization
Sample Identification and
Characterization

 Combustibility and deflagration characteristics heavily

influenced by:
• particle size distribution,
• particle morphology
• moisture content
 Highly sample specific and not material specific.
• Historical and literature data limited validity.
 Identify materials that should be studied; next review the
facility layout information process flow information to develop
a documented sampling plan. [multiple locations]
 These samples should then be uniquely identified so that they
can be traced back to a specific location.
 ASTM and NFPA recommend sub 75µm and 5% moisture.
 STAGE 3a:
Reactive as a Cloud
(Deflagration)
Go/No Go Explosibility Screening

 Modified Hartmann Tube Apparatus

• VDI 2263 Part 1 “Dust Fires and Dust
Explosions Hazards – Assessment –
Protective Measures: Test Methods for
the Determination of the Safety
Characteristics of Dusts”
• ISO/IEC 80079 -20-2 “Explosive
atmospheres – Part 20-2: Material
characteristics – Combustible dusts test
methods”.
 Spherical apparatus 20-L or 1-m³
• ASTM E1226 Section 13,
• VDI 2263 Part 1
• ISO/IEC 80079 -20-2
• CEN/CENELEC

10
Go/No Go Explosibility Screening

 Closed Chamber
- Vary concentration
- Use a strong ignition
source (5 or 10 kJ)
- Watch to see if peek
pressure exceeds the
“explosion” criterion.

11
 Stage 3b:
Reactive as a Pile or Layer
(Combustion)
Burning Behavior/Burn Rate
Screening

 Burning Behavior test

- VDI 2263 Part 1
- Mold powder into a pile using a
standard form
- Flame or platinum wire ignition
source
 Watch for propagation – Classify
 Burn Rate screening test
- UN Transportation of Dangerous
Goods test method
- Similar method but longer mold
 Watch for propagation

13
 STAGE 4a:
Deflagration Testing
Explosion Severity (Pmax & KSt)

 Determined in a 20-L or 1-m³ chamber

 Indication of the severity of an explosion
 Data used in the design of explosion protection devices
- Pmax = maximum pressure
- KSt = (dP/dt)max × V⅓

15
Explosion Parameters as a
Function of Dust Concentration

 Peak explosion data plotted as a  Rate of pressure rise data plotted

function of dust concentration as a function of dust concentration
 The highest point is the Pmax  The highest point is the (dP/dt)max
 In this graph for niacin, the Pmax  In this graph for Niacin, the
is 7.9 bar(g) at 500 g/m³ (dP/dt)max is 930 bar/s

16
Data Interpretation Tips

 Identify what apparatus is being used.

- 20L Vessel has potential for under-driving & over-driving
- Bureau of Mines Chamber only adequate for determining if a
material is explosible
 If over-driving is suspected consider 1m3 Challenge Test
- Low KSt <50 bar-m/s
- Low Pmax <3 bar

17
Minimum Explosible Concentration
(MEC)

 Lowest dust concentration that will

propagate an explosion
- Analogous to the Lower Flammability
Limit (LFL) for gas/air mixtures
- The lower the number, the less
dispersed dust required for a dust
deflagration
- Industrial hygiene levels lower than
explosible range
- Dust deposits are above explosible
range, but may move down
- MEC concentrations achievable if dust
is present in large quantities

18
Limiting Oxygen Concentration (LOC)

 Minimum quantity of oxygen required to propagate an

explosion
- Dust concentration independent
- Data can be used to develop an inerting strategy
- Start at optimal concentration
- Once established, test several other concentrations to verify

 Limiting the oxygen concentration of the air surrounding the

dust is a method of explosion control

19
Minimum Ignition Energy (MIE)

 Predicts the ease and likelihood of ignition of a dispersed

dust cloud
 MIE of a flammable dust is the minimum spark energy
needed to ignite an ideal concentration under lab conditions
- A capacitive discharge spark is used for this test
- Test can be run with or without inductance
- Compared to typical ES ignition sources

20
Minimum Ignition Temperature
of a Dust Cloud (MIT)

 Measures the sensitivity to

hot surfaces and
environments
- Hot surfaces in dryers,
bearings and mechanical
parts
- Friction spark ignition with
MIE data
- Maximum exposure
temperature

21
 STAGE 4b:
Combustion Testing
Burn Rate Test

 UN Manual of Tests and Criteria

for Transportation of Dangerous
Goods, Section 33, Classification
Procedures, Test Methods and
Criteria Relating to Class 4, Test
N.1: Test Method for Readily
Combustible Solids

23
Layer Ignition Temperature (LIT)
ASTM E2021

 Sensitivity to ignition on hot

surfaces
- Other side room temperature
 Longer exposure time
(1 - 2 hr)
- LIT is typically lower than MIT
• Some materials melt before
reacting
- Not a true minimum since layer
thickness affects results

24
Auto Ignition Screening
(Grewer)
 VDI2263 Part 1 Section 1.4.1
 Sample in 8-ml mesh basket
 Ramp at a constant rate of 1.2 °C
per minute up to a temperature of
300 °C.
 The air flow through the oven is
adjusted to a constant rate of 2 L
per minute.
 Sample temperature is monitored to
determine temperature rise above
that of the oven itself.
 Ignition - temperature in the bulk
powder temperature rises
significantly above the oven
temperature.
25
Hot Storage Screening

 VDI2263 Part 1 Section 1.4.2.

 Isothermally in a drying oven
• preheated fresh air at a rate of 100
L/h
 100 ml, 1000 ml, and 1600 ml
• but other sizes like 25 ml, 50 ml, and
500 ml
 Rise in temperature above that of
the storage temperature is
categorized as self-heating – or
400°C.
 Highest temperature tested that
does not ignite the sample is taken
to be the autoignition temperature
 Plot log V vs 1/T – scale to larger
volumes

26
Exothermic Decomposition Screening

 ASTM E2550 “Standard Test Method for Thermal

Stability by Thermogravimetry”
 ASTM E537 “Standard Test for the Thermal Stability of
Chemicals by Differential Scanning Calorimetry”
 Ambient to 1000°C on an ~5-mg sample.

 Thermograph and mass loss analyzed for endotherms

and exotherms.
 Screen for reactivity in a small
Size: 16.1343 mg

120 20

scale 100 15

80 10

Heat Flow (W/g)

Weight (%)

74.09%
60 5

40 0

20 -5

0 -10
0 200 400 600 800 1000
Exo Up Temperature (°C)

27
Smoldering Gas Evolution (Lütolf)

 VDI2263 Part 1 Section 1.5.1.

 Exothermic decomposition in O2 limited environments.
 ~2 g of sample used.
 Initial screening run at a 2.5°C/min ramp
 Series of isothermal tests if temperature rise is observed.
 Can also be used to determine if flammable gases generated
during decomposition reaction.

28
In Closing

 Proposed testing sequence tree.

- “A method and not the method.”
 Variables effecting output
- Dust properties
• (type, size and exposed surface area)
- Nature of oxidative atmosphere
• (sensitivity to oxygen or other oxidizer)
- Dispersion mechanisms
• (lofting of powder – light or fine powders stay lofted)
- Type / magnitude & location of ignition
• (low energy ignition or self ignition – fine powder)
- Nature of confinement
• (volume, yield strength and initial pressure)

29
End