ASTM E1387-95
(Test Method)Standard Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography
Standard Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography
SCOPE
1.1 This test method covers the identification of residues of ignitable liquids in extracts from fire debris samples. Extraction procedures are described in the referenced documents.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific precautionary statement, see 6.3.
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Designation: E 1387 – 95
AMERICAN SOCIETY FOR TESTING AND MATERIALS
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Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Ignitable Liquid Residues in Extracts from Fire Debris
Samples by Gas Chromatography
This standard is issued under the fixed designation E 1387; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Summary of Test Method
1.1 This test method covers the identification of residues of 3.1 The sample extract or preparation is introduced into the
ignitable liquids in extracts from fire debris samples. Extrac- gas chromatographic column containing a liquid phase suitable
tion procedures are described in the referenced documents. for the separation of common ignitable liquid components. The
1.2 The values stated in SI units are to be regarded as the resulting chromatogram is interpreted by techniques of pattern
standard. The values given in parentheses are for information recognition and pattern comparison described in this test
only. method. Ignitable liquids may fall into one of five major
1.3 This standard does not purport to address all of the classifications, or into a “miscellaneous” category described
safety concerns, if any, associated with its use. It is the herein.
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For a specific 4.1 The identification of an ignitable liquid residue in a
sample of fire debris can support a field investigator’s opinion
precautionary statement, see 6.3.
regarding the incendiary nature of a fire.
2. Referenced Documents
4.1.1 The identification of an ignitable liquid residue in a
2.1 ASTM Standards: fire scene does not necessarily lead to the conclusion that a fire
E 260 Practice for Packed Column Gas Chromatography was incendiary in nature. Further investigation may reveal a
E 752 Practice for Safety and Health Requirements Relating legitimate reason for the presence of ignitable liquids.
to Occupational Exposure to Carbon Disulfide 4.2 Due to the volatility of ignitable liquids and to variations
E 1385 Practice for Separation and Concentration of Ignit- in sampling technique, the absence of detectable quantities of
able Liquid Residues from Fire Debris Samples by Steam ignitable liquid residues does not necessarily lead to the
Distillation conclusion that ignitable liquids were not present at the fire
E 1386 Practice for Separation and Concentration of Ignit- scene.
able Liquid Residues from Fire Debris Samples by Solvent 4.3 When the gas chromatographic pattern is not sufficiently
Extraction complex, as described in 10.3, additional analytical techniques
E 1389 Practice for Cleanup of Fire Debris Sample Extracts are required.
by Acid Stripping
5. Apparatus
E 1412 Practice for Separation and Concentration of Ignit-
5.1 Gas Chromatograph—A chromatograph equipped with
able Liquid Residues from Fire Debris Samples by Passive
Headspace Concentration a flame ionization or mass spectral detector may be used. Other
detectors may be used if it can be shown that they have
E 1413 Practice for Separation and Concentration of Ignit-
able Liquid Residues from Fire Debris Samples by Dy- sensitivity and selectivity equal to the above detectors.
5.1.1 Sensitivity—The system shall be capable of detecting
namic Headspace Concentration
E 1618 Guide for Ignitable Liquid Residues in Extracts 0.05 volume % in carbon disulfide (or any appropriate solvent)
of any common ignitable mixtures.
from Fire Debris Samples by Gas Chromatography-Mass
Spectrometry 5.1.2 Sample Inlet System—A sample inlet system that
allows a reproducible volume of liquid to be injected.
5.1.3 Column—A non-polar capillary column is recom-
This test method is under the jurisdiction of ASTM Committee E-30 on
mended, but any column may be used provided that, under the
Forensic Sciences and is the direct responsibility of Subcommittee E30.01 on
conditions of use, the test mixture can be resolved into its
Criminalistics.
component peaks.
Current edition approved Oct. 10, 1995. Published December 1995. Originally
published as E 1387 – 90. Last previous edition E 1387 – 90. 5.1.3.1 The test mixture shall consist of equal parts by
Annual Book of ASTM Standards, Vol 14.02.
weight of the even-numbered normal alkanes ranging from
Annual Book of ASTM Standards, Vol 11.03.
E 1387
n-hexane through n-eicosane, plus the following aromatic change composition. Extracts in carbon disulfide may be
components: toluene, p-xylene, o-ethyltoluene, covered with water prior to removing the extracts from the
m-ethyltoluene, and 1,2,4-trimethylbenzene. sample preparation hood. Alternatively, septum seal vials may
5.1.3.2 If total resolution of the test mixture cannot be be used for storing any solvents or extracts.
obtained on a single column or program, changing columns or 7.2.1 If water is used as a sealant, exercise care to avoid the
programs is permitted as long as using both columns or introduction of water onto DMCS treated columns.
programs results in the complete resolution of the test mixture. 7.2.2 Avoid the use of water as a sealant if the presence of
5.2 Column Oven—A column oven capable of reproducible water soluble compounds is suspected.
temperature and temperature program settings in the range of
8. Calibration
50 to 300°C should be used.
5.3 Strip Chart Recorder—A recording potentiometer with 8.1 Calibrate the chromatographic instrument frequently
using standards of known concentrations of known ignitable
a full scale deflection of 10 mV or less should be used. The full
scale response of the recorder should not exceed 1 s. An liquids as well as blanks. Optimize gas flows periodically.
Refer to Practice E 260 for detailed instructions on operation of
integrator, or computerized data station and printer which
meets or exceeds these requirements, is acceptable. the gas chromatograph.
8.1.1 Run appropriate blanks and controls periodically.
5.4 Syringes:
5.4.1 For liquid samples—a microsyringe, capable of repro- 8.1.1.1 Clean syringes thoroughly between injections.
8.1.2 Run known standards as necessary.
ducibly introducing sample sizes in the range of 0.1 to 10.0
mL. 8.1.2.1 Standard chromatograms must be run under the
5.4.2 For gas samples—a gas-tight syringe capable of same chromatographic conditions as those used to produce the
sample chromatogram.
reproducibly introducing sample sizes in the range of 0.5 to 5
mL. 8.1.2.2 Every case file that includes a positive identification
of an ignitable liquid or residue must include the standard
6. Reagents and Materials
chromatogram used to confirm the identification.
8.2 Chromatogram Evaluation—A good chromatogram for
6.1 Purity of Reagents—Reagent grade chemicals shall be
comparison work is one in which the peaks of interest are 50
used in all tests. Unless otherwise indicated, it is intended that
to 100 % of full scale. Rerun samples, or replot chromatogram,
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where using different parameters (attenuation or sample size) to
achieve a good chromatogram.
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently 8.2.1 In addition to the chromatogram described above, it is
sometimes necessary to produce other, off-scale plots, in order
high purity to permit its use without lessening the accuracy of
the determination. to bring some features into view for comparison. Such off-scale
plots may be required when there are one or more components
6.2 Solvents—The solvent in which the extract is dissolved
will depend upon the extraction technique employed. Fre- present at a significantly higher concentration than the other
components in the residue.
quently check solvents for purity by running appropriate
blanks, both neat and evaporated, to at least twice the extent
9. Petroleum Distillate Classification System
used in the analysis.
9.1 Six major classes of complex liquid products are recog-
6.2.1 If Carbon disulfide is used, read and follow the safety
nized as usually identifiable by GC patterning alone when
precautions described in Practice E 752.
recovered from fire debris.
6.3 Carrier Gas—Caution: hydrogen, helium, and nitrogen
9.1.1 This test method is only intended to allow isolated
are compressed under high pressure, and hydrogen is an
residues to be characterized as to one of the types of products
extremely flammable gas.
listed in Table 1. Other characterizations of samples may be
6.4 Combustion Gases—Air and hydrogen (if a flame ion-
possible, but are not within the scope of this test method.
ization detector is used).
6.5 Activated Charcoal.
10. Procedure
7. Sample Handling
10.1 Obtain a chromatogram of the fire debris sample
extract.
7.1 Methods of obtaining the extracts or preparations for
10.2 Obtain a chromatogram of a matching, or nearly
analysis are described in Practices E 1385, E 1386, E 1389,
matching, standard, and compare the pattern of peaks visually.
E 1412, and E 1413.
10.2.1 The essential requirement for making a classification
7.2 Due to the volatility of the solvents and the analytes,
using this procedure is the matching of the sample chromato-
take care to ensure that samples do not evaporate or otherwise
gram with a known standard chromatogram obtained under
similar conditions, noting sufficient significant points of corre-
lation or similarities. Make all comparisons using only good
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
chromatograms, as described in 8.2.
listed by the American Chemical Society, see Analar Standards for Laboratory
10.2.2 Pattern matching requires that the entire pattern used
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
for comparison be displayed at the same sensitivity.
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD. 10.2.2.1 To provide sufficient detail for some comparisons,
E 1387
TABLE 1 Ignitable Liquid Classification System
“Peak Spread” Based on
Class Number (Class Name) N-Alkane Carbon Numbers Examples
(Unevaporated Liquid)
1 C –C Petroleum ethers, Pocket lighter fuels, Some rubber cement solvents, Skelly solvents,VM&
4 11
Light Petroleum Distillates (LPD) P Naphtha, Some camping fuels
2 C –C All brands and grades of automotive gasoline, including gasohol.
4 12
Gasoline
3 C –C Mineral spirits, Some paint thinners, Some charcoal starters, “Dry-cleaning” solvents, Some
8 12
Medium Petroleum Distillates (MPD) torch fuels, Some solvents for insecticides and polishes, some lamp oils
4 C –C Number 1 Fuel Oil, Jet-A (aviation) fuel, Insect sprays, Some charcoal starters, Some torch
9 17
Kerosene fuels, Some paint thinners, Some solvents for insecticides and polishes, some lamp oils
5 C –C Number 2 fuel oil, Diesel fuel
9 23
Heavy Petroleum Distillates (HPD)
Miscellaneous Variable Single compounds, Turpentines, Specialty mixtures that cannot be further classified into one
of the categories below
0.1
Oxygenated solvents Variable Alcohols, Esters, Ketones
0.2
Isoparaffins Variable Isoparaffin products, Some charcoal starters, Some copier fluids, Some aviation gasolines,
Some lamp oils, Some solvents for insecticides and polishes, Some camping fuels
0.3
Normal alkanes Variable Specialty products formulated from normal alkanes, Some lamp oils, Some solvents for
insecticides and polishes
0.4
Aromatic solvents Variable Light, medium and heavy “aromatic naphtha” used as solvents for paints and plastics
0.5
Naphthenic/paraffinic solvents Variable Specialty solvent/fuel products made from Class 3 or Class 4 distillates-treated to remove
normal alkanes and aromatics, with higher cycloalkane content than isoparaffin products
different amplitudes or presentations of the data may be 10.3 Use the following criteria to determine whether suffi-
necessary. cient similarities exist between the sample and the standard to
10.2.2.2 The carbon number range is determined by com- classify the residue:
paring the chromatogram to a standard containing known 10.3.1 . Class 1—At least four major peaks matching a
normal alkanes, as shown in Fig. 1. known Class 1 standard are in the C to C range. No major
4 11
10.2.3 Store the standard chromatogram(s) in the case file, peak beyond C is associated with ignitable liquids. Examples
along with the sample chromatogram(s). of Class 1 liquids are shown in Fig. 2 and Fig. 3.
Chromatographic Conditions
Instrument: HP 5890 Gas Chromatograph Initial Temperature: 60°C, 6 min
Detector: HP 5971 Mass Selective Detector Ramp: 20°C/min
Column: 25 m, HP-1, 0.2 mm, ID, 0.5 μm film thickness Final Temperature: 280°C, 4 min
All injections are 1 μL of a 1 % solution in diethyl ether.
NOTE 1—These are typical chromatograms, provided for illustration only. Each laboratory is likely to obtain slightly different retention times and
relative abundances of individual components, depending on sample history, separation procedure, and chromatographic conditions.
FIG. 1 C –C Normal Alkanes
6 20
E 1387
Chromatographic Conditions
Instrument: HP 5890 Gas Chromatograph Initial Temperature: 60°C, 6 min
Detector: HP 5971 Mass Selective Detector Ramp: 20°C/min
Column: 25 m, HP-1, 0.2 mm, ID, 0.5 μm film thickness Final Temperature: 280°C, 4 min
All injections are 1 μL of a 1 % solution in diethyl ether.
NOTE 1—These are typical chromatograms, provided for illustration only. Each laboratory is likely to obtain slightly different retention times and
relative abundances of individual components, depending on sample history, separation procedure, and chromatographic conditions.
FIG. 2 Example of a Class 1 Pattern; Brand A Cigarette Lighter Fluid
Chromatographic Conditions
Instrument: HP 5890 Gas Chromatograph Initial Temperature: 60°C, 6 min
Detector: HP 5971 Mass Selective Detector Ramp: 20°C/min
Column: 25 m, HP-1, 0.2 mm, ID, 0.5 μm film thickness Final Temperature: 280°C, 4 min
All injections are 1 μL of a 1 % solution in diethyl ether.
NOTE 1—These are typical chromatograms, provided for illustration only. Each laboratory is likely to obtain slightly different retention times and
relat
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