F I R E & S M O K E D A M A G E T E S T I N G 1

2 E M S L A N A L Y T I C A L , I N C . P O C K E T G U I D E
 Table of Contents
Fire & Smoke Damage Testing 4-5
(Char, Ash, Black Carbon/Soot)

Air Sampling 6 - 10

Surface Sampling 11 - 20

Analytical Options 21 - 29

Methods for Deriving Concentrations 30 - 32

Additional Information 33 - 34

F I R E & S M O K E D A M A G E T E S T I N G 3
Fire & Smoke Damage Testing
(Char, Ash, Black Carbon/Soot)
The purpose of this guide is to provide information regarding the typical
sampling and analytical procedures involved in fire debris investigations. The
components of fire debris are complex and their nature depends on the type of
materials involved in the fire, the combustion conditions, and the presence of
fuels/accelerators. In general, the common by-products of fires can be classified
in three categories: char, ash, and soot/black carbon.
Char is defined in ASTM D6602-13 as particulate larger than 1 μm made by
incomplete combustion which may not deagglomerate or disperse by ordinary
techniques, may contain material which is not black, and may contain some of
the original material’s cell structure, minerals, ash, cinders, and so forth. Carbon
is typically the predominant component in char.
Ash is pyrolized material obtained from advanced combustion of char. Because the
carbon matrix of char is almost completely combusted, ash has a minerals-based
matrix, with a high amount of elements such as calcium, potassium, magnesium,
aluminum, silicon, phosphorus or sulfur. The particles are very brittle and may
or may not contain some of the original material’s cell structure.
Soot is defined in ASTM D6602-13 as submicron black powder generally
produced as an unwanted by-product of combustion or pyrolysis. It consists
of various quantities of carbonaceous and inorganic solids in conjunction
with adsorbed and occluded organic tars and resins. The EPA defines
black carbon as the sooty black material emitted from gas and diesel engines,
coal-fired power plants, and other sources that burn fossil fuel.
Carbon black is a term usually associated with soot, although they are different
materials and have distinctively different origins. Carbon black is an engineered,

4 E M S L A N A L Y T I C A L , I N C . P O C K E T G U I D E
industrially produced material, primarily composed of elemental carbon,
obtained from the partial controlled combustion or thermal decomposition
of hydrocarbons (most hydrocarbons are found in crude oil and other fuels).
Soot/black carbon and carbon black terms should not be used interchangeably.
The most important characteristics of soot/black carbon and carbon black
particles are their size range and the aciniform morphology. Aciniform carbon
is colloidal carbon having a morphology consisting of spheroidal primary
particles (nodules) fused together in aggregates of colloidal dimension in a
shape having grape-like clusters or open branch-like structures.

The Main Differences Between Soot/Black Carbon

and Carbon Black are:
• For carbon black, the particle size and aggregate size vary depending
on the carbon black grade; while particle and aggregate sizes vary greatly
within a given grade of carbon black, the primary particle size is essentially
uniform within an individual aggregate.
• Soot/black carbon may have several carbon morphologies depending
on the source; the particle size range is wide and non-uniform.
• Carbon black grades are quite low in volatile organic content (<8 %)
whereas soot/black carbon is normally high in volatile organic
content (>20 %).
• Soot/black carbon contains minerals, residual tars and resins where
carbon black may contain trace amounts of hydrocarbons used as
precursors.

F I R E & S M O K E D A M A G E T E S T I N G 5
Air Sampling
Air sampling for combustion by-products
Option 1: Gravimetric analysis based on
NIOSH 5000- Carbon Black
Sampler: tared 5-µm PVC membrane
Flow rate: 1-2 Liter/min
Min Volume: 30 Liters at 3.5 mg/m3
Max Volume: 570 Liters
Results expressed in mg/m3 as carbon black
Advantages
Pre-Weighted/Tared
• Quick and simple procedures. 37 mm 5 µm
• Analysis is simple. PVC Cassette
Disadvantages:
• Analysis is non-specific. The presence of any other particulate material
in the air being sampled will be a positive interference since this is a
gravimetric method. Information on any other particulate materials
present should be assessed, by using electron microscopy for example.
• Sampling requires an air sampling pump and air sampling cassettes.
• The sample represents the particles present in the air at the time of
collection.
Sampling Procedure
• Calibrate each personal sampling pump with a representative sampler
in line. Sample at 1 to 2 L/min for a total sample volume of 30 to 570 L.
Do not exceed a filter loading of approximately 2 mg total dust. Take two
to four replicate samples for each batch of field samples for quality
assurance on the sampling procedures.

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 • Remove the cassette from the sampling tubing.
• Complete the applicable EMSL Chain of Custody (COC), detailing
client name and information, project name or number, sample #,
description of area, and volume of air collected.
• Ship the samples along with COC to the laboratory.

Option 2: PCM or TEM Cassettes

(based on NIOSH 7400 sampling method)
Sampler: 0.45 to 1.2 µm mixed cellulose ester membrane
(MCE), 25 to 37 mm diameter
Flow rate: 0.5-16 Liter/min
Min Volume: 400 liters
Max Volume: 1000-1200 liters
Results expressed in one of the options below:
• Particles/liter
• Particles/cm3

• Particles/m3 0.8 µm Mixed Cellulose
• % Particles (by point count procedures) Ester Membrane (MCE),
25 mm Diameter
Advantages
• Able to determine the amount of target analytes present in the air at
the time of collection, derived by particle count.
Disadvantages:
• The sample represents the particles present in the air at the time of
collection; therefore collection is representative if the combustion
event is current.

F I R E & S M O K E D A M A G E T E S T I N G 7
 • Sampling requires pump and cassettes.
• Analysis provides full char and ash analysis; the soot/black carbon
analysis is presumptive only.
Sampling Procedure
• Calibrate each personal sampling pump with a representative sampler in
line. To reduce contamination and to hold the cassette tightly together,
seal the crease between the cassette base and the cowl with a shrink band
or light colored adhesive tape.
• Submit at least one field blank (or 10% of the total samples, whichever
is greater) for each set of samples. Handle field blanks in a manner
representative of actual handling of associated samples in the set.
Open field blank cassettes at the same time as other cassettes just
prior to sampling.
• Store top covers and cassettes in a clean area (e.g., a closed bag or box)
with the top covers from the sampling cassettes during the sampling
period.
• Sample at 0.5 L/min or greater.
• Remove the cassette from the sampling tubing after sampling.
• Complete the applicable EMSL Chain of Custody (COC), detailing
client name and information, project name or number, sample #,
description of area, and volume of air collected.
• Ship the samples along with COC to the laboratory.

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Option 3: Air-O-Cell
Sampler: Air-O-Cell cassette
Flow rate: 15 Liter/min
Min Volume: 15 liters (dusty environment)
Max Volume: 150 liters
(no visible dust, “clean” environment)
Typical volume: 75 liters
Results expressed in one of the options below:
• Particles/liter
AIR-O-Cell Cassette
• Particles/m3
• Particles/cm3
Advantages
• Quick and simple procedures.
• Analysis is simple.
• Able to determine the amount of target analytes present in the
air at the time of collection, derived by particle count.
Disadvantages
• The sample represents the particles present in the air at the time of
collection; therefore, collection is representative if the combustion
event is current.
• Sampling requires an air sampling pump and air sampling cassettes.
• Analysis provides full char analysis; ash analysis may be hindered due
to the presence of adhesive on the trace; the soot/black carbon analysis
is presumptive only.

F I R E & S M O K E D A M A G E T E S T I N G 9
Sampling Procedure
• Prior to sampling, calibrate the pump at 15 liters/min with a rotameter.
• Remove and retain the tape seal covering inlet and outlet on the cassette.
• Attach the outlet (round hole) to a standard ½” PVC tubing
(for use with high volume pumps only).
• Start the sampling pump and sample for an appropriate amount of time.
• Remove Air-O-Cell from tubing and reseal.
• Complete the applicable EMSL Chain of Custody (COC), detailing
client name and information, project name or number, sample #,
description of area, and volume of air collected.
• To reduce shipping damage, it is recommended that the Air-O-Cell be
placed in a corrugated box with padding to ensure safe arrival at the
laboratory.

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Surface Sampling
Surface sampling for combustion by-products

Option 1: Micro Vacuuming

Micro-vacuum (micro-vac) sample collection involves the use of air filter
cassettes. Commonly, MCE filter cassettes are attached to high volume pumps
in the same manner as air sampling. A Closed Face cassette setup is used in
order to attach a short length of tubing to the sampling inlet. The particulate
is then collected by crisscrossing the sampling area with the collection tube.

Carpet Sample Kit Micro-Vac Cassette Options

F I R E & S M O K E D A M A G E T E S T I N G 11
 Micro-Vacuuming Tubing Set-Up

Advantages
• Able to determine the amount of target analytes present on
surfaces during or after the event.
• Very efficient sampling method for collecting particles from porous,
uneven or difficult to access places with medium and heavy loading
(rugs, fabrics and collection vents, narrow grills or cracks).
• The samples represent bulk amount of particle material, often of
many different sizes.
• A variety of optical and electron microscopy methods can be used
in the identification analysis.
• Confirmatory identification of aciniform soot by Transmission
Electron Microscopy (TEM), as mandated in ASTM D6602-13,
can be applied using the drop-mount technique.

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 • Chemical analysis of organic compounds associated with the fire
deposits through bulk spectroscopy and/or chromatography
(such as PAH’s) can be applied.
• Corrosivity analysis via pH measurement or anions scan by Ion
Chromatography can be applied.

Disadvantages
• Sampling requires an air sampling pump and air sampling cassettes.
• Poor efficiency for collecting particles from relatively smooth
non-porous surfaces with low loading.
• It does not preserve the relative positions of the particles on the
original surface and the population per unit area; however, this is
a limitation only when the agglomerate size and the distribution
over the collection surface is of interest.
• Can induce damage to brittle particles such as char and ash; if
proper sampling and sample preparation procedures are applied,
the damage can be greatly minimized.

Recommended surfaces for sampling

Main living areas, interior of door frame, corner of floors; door tracks;
attic areas; soft surfaces, wood, upholstery, clothing.

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 Option 2: Tape Lifting
(Forensic Adhesive Lifts, Transparent Office Tape)
Advantages
• Quick and simple sampling procedures.
• Able to determine the amount of target analytes present on surfaces
during or after the event.
• Efficient sampling method for collecting particles from relatively
smooth non-porous surfaces with typical monolayer loading
(desks, furniture, glass and hard floors).
• Preserves the relative positions of the particles on the original
surface and the population per unit area.
• A variety of optical microscopy methods can be used in the
identification analysis, with minimal preparation.
• Scanning Electron Microscopy/Energy Dispersive X-rays (SEM/EDX)
methodology can be applied for comprehensive characterization of
char and ash and presumptive identification of soot clusters.

Disadvantages
• Poor efficiency for collecting on porous, uneven or heavily loaded
surfaces, showing preferential sampling from the top layer particles.
• Application of overpressure during sampling can obscure or damage
the brittle particles of char and ash.

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 Forensic Tape Lift (Instant Tape Lifters)

Tape Lift (Transparent/Clear Tape)

F I R E & S M O K E D A M A G E T E S T I N G 15
 • Limited sampling area.
• Particles that are part of large agglomerations many not be correctly
identified by applicable methods due to overlapping.
• Confirmatory identification of aciniform soot by Transmission
Electron Microscopy (TEM), as mandated in ASTM D6602-13,
cannot be applied.
• Chemical analysis of organic compounds associated with the fire
debris through spectroscopy and/or chromatography (such as PAH’s)
cannot be applied.
• Corrosivity analysis via pH measurement or anions scan by Ion
Chromatography cannot be applied.

Note: Packing tape should be avoided since these products have a thick layer
of adhesive that can trap particles hence hindering analysis. Non-transparent
and industrial tapes, such as duct tape cannot not be used.

Recommended surfaces for sampling

Main living areas, interior of door frame, corner of floors, door tracks,
attic areas.

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Option 3: Wet Wiping/Alcohol Prep Wipes
Unlike Ghost Wipes, paper towels and commercial products such as
Wet-Wipes™, alcohol pads have a small surface area so particles are easily
extracted for analysis. Particles tend to become trapped in larger wipes
and paper products often interfering with accurate analysis. Avoid using
water-based moistening agents as many common particles are water soluble.

Alcohol Prep Wipes

Advantages
• Quick and simple sampling procedures.
• Efficient sampling method for collecting particles from relatively
smooth non-porous surfaces with low or heavy loading.

F I R E & S M O K E D A M A G E T E S T I N G 17
 • A variety of optical and electron microscopy methods can be used in
the identification analysis.
• Confirmatory identification of aciniform soot by Transmission Electron
Microscopy (TEM), as mandated in ASTM D6602-13, can be applied
using the drop-mount technique.
• Particle dispersion techniques for breaking up the agglomerates enables
more accurate identification of individual grains, necessary when
environmental interferences are suspected.
• Chemical analysis of organic compounds associated with the fire
deposits through bulk spectroscopy and/or chromatography
(such as PAH’s) can be applied.
• Corrosivity analysis via pH measurement or anions scan by Ion
Chromatography can be applied.

Disadvantages
• Poor efficiency for collecting on porous and uneven surfaces.
• It does not preserve the relative positions of the particles on the
original surface and the population per unit area; however, this is
a limitation only when the agglomerate size and the distribution
over the collection surface is of interest.
• Can induce damage to brittle particles such as char and ash.

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 • There can be variance in what particles are successfully transferred
from the wipe and therefore isolated for analysis.

Recommended surfaces for sampling

TVs, computer displays, plastic surfaces, furniture, windows, refrigerators.
Note: avoid painted surfaces due to transfer of the paint on the wipe.

Option 4: Bulk/ Grab Sample

Abundant deposits are generally treated as bulk when sampling. Sampling
consists of transferring the material/fire debris to a zip-lock style bag or rigid
container. Sampling may be performed by glove-bag, trowel, scraping the
material into a pile or any other technique available.

Advantages
• Quick and simple sampling procedures.
• Efficient sampling method for collecting particles from various surfaces
with heavy loading.
• A variety of optical and electron microscopy methods can be used in
the identification analysis.
• Confirmatory identification of aciniform soot by Transmission Electron
Microscopy (TEM), as mandated in ASTM D6602-13, can be applied
using the drop-mount technique.

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 • Particle dispersion techniques for breaking up the agglomerates enables
more accurate identification of individual grains, necessary when
environmental interferences are suspected.
• Chemical analysis of organic compounds associated with the fire
deposits through bulk spectroscopy and/or chromatography
(such as PAH’s) can be applied.
• Corrosivity analysis via pH measurement or anions scan by Ion
Chromatography can be applied.

Disadvantages
• Poor efficiency on surfaces with light loading.
• It does not preserve the relative positions of the particles on the
original surface and the population per unit area; however, this is
a limitation only when the agglomerate size and the distribution
over the collection surface is of interest.
• Can induce damage to brittle particles such as char and ash.

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Analytical Options
Based on the identity and characteristics of the particulate components present
in fire debris, the main analytical techniques used for identification are:

• Light Microscopy
Stereomicroscopy
Reflected Light Microscopy
Polarized Light Microscopy

• Transmission Electron Microscopy with Energy

Dispersive X-Ray
(TEM/EDX)

• Scanning Electron Microscopy with Energy

Dispersive X-Ray
(SEM/EDX)

Each of these techniques provides the means to observe

and characterize specific fingerprinting traits of the
target analytes in fire residues.

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Stereomicroscopy
• It provides relatively low magnification observation and it gives the
possibility of three dimensional observation of the components in the
sample due to focusing on the same point from two different angles.
• It is used for initial examination of surface and bulk samples to observe
the overall aspect of the components and the presence of large particulate.
• During the analysis by Stereomicroscope, the sample is analyzed to
observe the characteristics of the particles such as color, size range,
morphology, and evidence of cellular morphology of char and ash.

Image of Stereo Microscope Stereo Image of Wood Char

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Reflected Light Microscopy (RLM)

• Primarily used to examine opaque particles: metals, coal/coke, wood,

slag, rock, plastics, alloys, composites, char.

• It is also used for initial examination of surface and bulk samples to observe
the overall aspect of the components and the presence of large particulate.

• Similar to Stereomicroscope, the analysis by RLM is also used to observe

the color, size range, morphology and evidence of cellular morphology of
char and ash.

Image of Reflected Light RLM image of Wood Char

Microscope

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 Polarized Light Microscopy (PLM)
• Light microscopy technique involving observation with polarized light.
• Polarized light is a contrast-enhancing technique that improves the
quality of the image obtained with birefringent materials.
• Identification is based on morphology, sign of elongation,
birefringence, pleochroism, angle of extinction, and refractive index.
• The PLM technique is used for full identification of char and ash
and screening/presumptive analysis of soot clusters.

Image of the Polarized Light PLM image of Wood Char and Ash
Microscope (PLM)

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Transmission Electron Microscopy with Energy Dispersive
X-Ray (TEM/EDX)
• High magnification electron microscopy technique using a beam of
high energy electrons transmitted through the specimen to create an
image; the additional X-rays produced in the interaction are used to
create elemental spectrum.
• This test method is a mandatory evaluation of soot/black carbon present
in the sample because the high magnification allows determining if the
morphology is consistent with grape-like or branchlike structures, the
size range of individual particles and the elemental composition (with
the EDX attachment).

Image of TEM/EDX Instrument TEM Image of Soot/Black Carbon; The

Size of Individual Particles is ~50 nm

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 Scanning Electron Microscopy with Energy Dispersive X-Ray
(SEM/EDX)
• Electron microscopy technique using a beam of high energy electrons
to bombard the specimen and extract secondary electrons from the
specimen to create an image; the additional X-rays produced in the
interaction are used to created elemental spectrum.
• This method is used to obtain morphological details and elemental
composition of char and ash; it can also be used for screening/
presumptive analysis of soot clusters.

TEM/EDX Spectrum of Soot/Black Carbon;

Copper Signal is Due to the TEM Copper
Grid used for Mounting

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 Image of SEM/EDX
Instrument

SEM Image of Wood Char

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 SEM/EDX Spectrum of Wood Char

SEM Image of Wood Ash

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 SEM/EDX Spectrum of Wood Ash

F I R E & S M O K E D A M A G E T E S T I N G 29
Methods for Deriving Concentrations
Air sample by NIOSH 5000
Gravimetric methods, similar to NIOSH 0500/0600 methods
Concentration, C (mg/m3) in the air volume sampled, V (L):

Where
W1 = Tare weight of filter before sampling (mg)
W2 = Post-sampling weight of sample-containing filter (mg)
B1 = Tare weight of blank filter (mg)
B2 = Post-sampling weight of blank filter (mg)

Air sample with MCE or Air-o-Cell cassettes

Particle Count Method
• Results expressed as “number of particles/volume of air”.
• Method does not take into consideration the particle size.

Surface or bulk/grab sample

A. Visual Area Estimation Method (defined in EPA 600/R-93/116)
• It estimates the relative projected area of a certain type of particulate
from a mixture of particulate by comparison to data derived from
analysis of calibration materials having similar texture and particulate
content.

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B. Point Count Method
• Results expressed as “%” area.
• The fraction of points within a rectangular grid superimposed on a
two-dimensional planar microscopic field provides an estimate for the
volume fraction of identifiable constituents.
• Method does take into consideration the particle size.

Recommendation
An effective interpretation of the results is based on the comparison with
unaffected areas. If possible, obtain a control sample from an area not
affected by fire to be used as background.

Analytical Packages (surfaces and bulk sampling)

Level Provided Analytes of Interest Analytical Techniques

by EMSL included in the Analysis Applied for Analysis
Analytical, Inc.
Screening • Char • Light Microscopy
• Ash (Stereo, RLM, PLM)
• Soot/Black Carbon • Presence/Absence;
(Presumptive/Screening) No Concentrations Reported
Level 1 • Char • Light Microscopy
• Ash (Stereo, RLM, PLM)
• Soot/Black Carbon • Concentrations of Analytes are
(Presumptive/Screening) Reported

F I R E & S M O K E D A M A G E T E S T I N G 31
Analytical Packages (surfaces and bulk sampling)

Level Provided Analytes of Interest Analytical Techniques

by EMSL included in the Analysis Applied for Analysis
Analytical, Inc.
Level 2 • Char • Light Microscopy
• Ash (Stereo, RLM, PLM)
• Soot/Black Carbon • TEM/EDX (for Soot/Black Carbon)
(confirmatory) • Concentrations of Analytes are
Reported
Level 3 • Char • Light Microscopy
• Ash (Stereo, RLM, PLM)
• Soot/Black Carbon • TEM/EDX (for Soot/Black Carbon)
• Common Components Of • SEM/EDX (for Overall Elemental
Environmental Dust: Composition of The Sample)
MMVF’s, Biological • Concentrations of Analytes Are
Components (Pollen, Mold), Reported
Cellulose, Synthetic Fibers,
Quartz, Calcite
Level 4 • Char • Light Microscopy
• Ash (Stereo, RLM, PLM)
• Soot/Black Carbon • TEM/EDX (for Soot/Black Carbon)
• Common Components of • SEM/EDX (for Elemental
Environmental Dust: Composition of Soot, Char,
MMVF’s, Biological and Ash)
Components (Pollen, Mold), • Concentrations of Analytes are
Cellulose, Synthetic Fibers, Reported
Quartz, Calcite pH • Value of pH and Comparison with
Blanks is Reported

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Additional Information
Recommendation
An effective interpretation of the results is based on the comparison with
unaffected areas. If possible, obtain a control sample from an area not
affected by fire to be used as background.

Soot Source Identification

• Analysis for presence of residual products consumed in fires by Gas
Chromatography-Mass Spectroscopy/GC-MS (such as aliphatic
hydrocarbons from fuels, phthalates from plastics, paraffin from
candles, Fatty Acids from edible oils, Levoglucosan from
carbohydrates/cellulose).
• Residual sulfur associated with Methyl Mercaptan, the olfactive
indicator from natural gas.
• Protein fires: analysis for Tryptophan and /or Albumin by Liquid
Chromatography - Tandem Mass Spectrometry (LC-MS/MS).

Corrosion propensity of fire residues when resting on metal surfaces

• pH measurement.
• Anions scan associated with non-volatile acids, determined by
Ion Chromatography/IC (chloride, fluoride, bromide, nitrate,
nitrite, phosphate, and sulfate).

F I R E & S M O K E D A M A G E T E S T I N G 33
Metallic Elements in fire residues
• Analysis by Inductively Coupled Plasma Mass Spectrometry
(ICP-MS) for target elements, including heavy metals.

Aldehydes and Volatile Organic Compounds (VOCs)

• Compounds associated with odors and toxic organics.
• TO-15 analysis of air collected in specially-prepared canisters
and analyzed by GC/MS.
• Aldehyde profile by HPLC (based on NIOSH 2016 method).

IESO/RIA Standard 6001

• Char is used as the primary indicator.
• Soot is used as the secondary indicator.
• It is a screening method.
• The method is not designed to provide identification of individual
char particles nor to determine the origin of soot particles.

References:
ASTM D6602-13-Standard Practice for Sampling and Testing of Possible Carbon
Black Fugitive Emissions or Other Environmental Particulate, or Both
EPA 600/R-93/116- Method for the Determination of Asbestos In Bulk Building
Materials
IESO/RIA Standard 6001-2011-Evaluation of HVAC Interior Surfaces to
Determine the Impact from Fire-related Particulate

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F I R E & S M O K E D A M A G E T E S T I N G 35
 ©2018 EMSL Analytical, Inc.

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