ASTM E2677-14
(Test Method)Standard Test Method for Determining Limits of Detection in Explosive Trace Detectors
Standard Test Method for Determining Limits of Detection in Explosive Trace Detectors
SIGNIFICANCE AND USE
5.1 ETDs are used by first responders, security screeners, the military, and law enforcement to detect and identify explosive threats quickly. ETDs typically operate by detecting chemical agents in residues and particles sampled from surfaces and can have detection limits for some compounds extending below 1 ng. An ETD is set to alarm when its response to any target analyte exceeds a programmed threshold level for that analyte. Factory settings of such levels typically balance sensitivity and selectivity assuming standard operating and deployment conditions.
5.2 A LOD is commonly accepted as the smallest amount of a particular substance that can be reliably detected in a given type of medium by a specific measurement process (2, 3). The analytical signal from this amount shall be high enough above ambient background variation to give statistical confidence that the signal is real. Methods for determining nominal LOD values are well known (for example, Hubaux and Vos (7) and Practice D6091), but pitfalls exist in specific applications. Vendors of ETDs often report detection limits for only a single compound without defining the meaning of terms or reference to the method of determination.Note 1—There are several different “detection limits” that can be determined for analytical procedures. These include the minimum detectable value, the instrument detection limit, the method detection limit, the limit of recognition, and the limit of quantitation. Even when the same terminology is used, there can be differences in the LOD according to nuances in the definition used, the assumed response model, and the type of noise contributing to the measurement.
5.3 When deployed, individual ETD performance (for example, realistic LODs) is influenced by: (1) ETD manufacturing differences, history, and maintenance; (2) ETD operating configurations (for example, thermal desorption temperature, analyzer temperature, and type of swab); and (3) environmental conditions (for exampl...
SCOPE
1.1 In harmony with the Joint Committee for Guides in Metrology (JCGM) and detection concepts of the International Union of Pure and Applied Chemistry (IUPAC) (1, 2, 3)2, this test method uses a series of replicated measurements of an analyte at dosage levels giving instrumental responses that bracket the critical value, a truncated normal distribution model, and confidence bounds to establish a standard for determining practical and statistically robust limits of detection to analytes sampled on swabs by explosive trace detectors (ETDs).
1.2 Here, the limit of detection (LOD90) is defined to be the lowest mass of a particular compound deposited on a sampling swab for which there is 90 % confidence that a single measurement in a particular ETD will have a true detection probability of at least 90 % and a true nondetection probability of at least 90 % when measuring a process blank sample.
1.3 This particular test method was chosen on the basis of reliability, practicability, and comprehensiveness across tested ETDs, analytes, and deployment conditions. The calculations involved in this test method are published elsewhere (4), and may be performed consistently with an interactive web-based tool available on the National Institute of Standards and Technology (NIST) site: http://pubapps.nist.gov/loda.
1.4 Intended Users—ETD developers, ETD vendors, ETD buyers, ETD testers, ETD users (first responders, security screeners, and the military), and agencies responsible for public safety and enabling effective deterrents to terrorism.
1.5 While this test method may be applied to any detection technology that produces numerical output, the procedures have been designed for ion mobility spectrometry (IMS) based ETD systems and tested with low vapor pressure explosive compounds. Compounds are deposited as liquid solutions on swabs and dried before use. As some swabs are absorbent, this deposition procedure may not be opt...
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Designation: E2677 − 14
Standard Test Method for
Determining Limits of Detection in Explosive Trace
1
Detectors
This standard is issued under the fixed designation E2677; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope deposition procedure may not be optimal for those ETD
technologies that rely on high coverage of analyte on the
1.1 In harmony with the Joint Committee for Guides in
surface of the swab. Background interferences introduced to
Metrology (JCGM) and detection concepts of the International
2 the test samples were representative of a variety of conditions
Union of Pure andApplied Chemistry (IUPAC) (1, 2, 3) , this
expected during deployment, but these conditions were not
test method uses a series of replicated measurements of an
intended as comprehensive in representing all possible sce-
analyte at dosage levels giving instrumental responses that
narios.Theusershouldbeawareofthepossibilitythatuntested
bracket the critical value, a truncated normal distribution
scenarios may lead to failure in the determination of a reliable
model, and confidence bounds to establish a standard for
LOD90 value.
determiningpracticalandstatisticallyrobustlimitsofdetection
to analytes sampled on swabs by explosive trace detectors 1.6 Units—The values stated in SI units are to be regarded
(ETDs). as the standard. No other units of measurement are included in
this standard.
1.2 Here, the limit of detection (LOD90) is defined to be the
1.7 This standard does not purport to address all of the
lowest mass of a particular compound deposited on a sampling
safety concerns, if any, associated with its use. It is the
swab for which there is 90 % confidence that a single mea-
responsibility of the user of this standard to establish appro-
surement in a particular ETD will have a true detection
priate safety and health practices and determine the applica-
probability of at least 90 % and a true nondetection probability
bility of regulatory limitations prior to use. Some specific
of at least 90 % when measuring a process blank sample.
hazards statements are given in Section 8 on Hazards.
1.3 This particular test method was chosen on the basis of
reliability, practicability, and comprehensiveness across tested
2. Referenced Documents
ETDs, analytes, and deployment conditions. The calculations
3
2.1 ASTM Standards:
involved in this test method are published elsewhere (4), and
D6091 Practice for 99 %/95 % Interlaboratory Detection
may be performed consistently with an interactive web-based
Estimate (IDE) for Analytical Methods with Negligible
tool available on the National Institute of Standards and
Calibration Error
Technology (NIST) site: http://pubapps.nist.gov/loda.
E177 Practice for Use of the Terms Precision and Bias in
1.4 Intended Users—ETD developers, ETD vendors, ETD
ASTM Test Methods
buyers, ETD testers, ETD users (first responders, security
E200 Practice for Preparation, Standardization, and Storage
screeners, and the military), and agencies responsible for
of Standard and Reagent Solutions for ChemicalAnalysis
public safety and enabling effective deterrents to terrorism.
E288 Specification for Laboratory Glass Volumetric Flasks
1.5 While this test method may be applied to any detection
E456 Terminology Relating to Quality and Statistics
technology that produces numerical output, the procedures E542 Practice for Calibration of Laboratory Volumetric
have been designed for ion mobility spectrometry (IMS) based
Apparatus
ETD systems and tested with low vapor pressure explosive E691 Practice for Conducting an Interlaboratory Study to
compounds. Compounds are deposited as liquid solutions on
Determine the Precision of a Test Method
swabs and dried before use.As some swabs are absorbent, this E969 Specification for Glass Volumetric (Transfer) Pipets
E1154 Specification for Piston or Plunger Operated Volu-
metric Apparatus
1
This test method is under the jurisdiction of ASTM Committee E54 on
Homeland Security Applications and is the direct responsibility of Subcommittee
E54.01 on CBRNE Sensors and Detectors.
3
Current edition approved Feb. 1, 2014. Published February 2014. DOI: 10.1520/ For referenced ASTM standards, visit the ASTM website, www.astm.org, or
E2677-14. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
The boldface numbers in parentheses refer to a list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
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