ASTM E594-96(2011)
(Practice)Standard Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
Standard Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
SIGNIFICANCE AND USE
Although it is possible to observe and measure each of the several characteristics of a detector under different and unique conditions, it is the intent of this recommended practice that a complete set of detector specifications should be obtained at the same operating conditions, including geometry, flow rates, and temperatures. It should be noted that to specify a detector's capability completely, its performance should be measured at several sets of conditions within the useful range of the detector. The terms and tests described in this recommended practice are sufficiently general so that they may be used at whatever conditions may be chosen for other reasons.
The FID is generally only used with non-ionizable supercritical fluids as the mobile phase. Therefore, this standard does not include the use of modifiers in the supercritical fluid.
Linearity and speed of response of the recording system or other data acquisition device used should be such that it does not distort or otherwise interfere with the performance of the detector. Effective recorder response, Bonsall (5) and McWilliam (6), in particular, should be sufficiently fast so that it can be neglected in sensitivity of measurements. If additional amplifiers are used between the detector and the final readout device, their characteristics should also first be established.
SCOPE
1.1 This practice covers the testing of the performance of a flame ionization detector (FID) used as the detection component of a gas or supercritical fluid (SF) chromatographic system.
1.2 This recommended practice is directly applicable to an FID that employs a hydrogen-air or hydrogen-oxygen flame burner and a dc biased electrode system.
1.3 This recommended practice covers the performance of the detector itself, independently of the chromatographic column, the column-to-detector interface (if any), and other system components, in terms that the analyst can use to predict overall system performance when the detector is made part of a complete chromatographic system.
1.4 For general gas chromatographic procedures, Practice E260 should be followed except where specific changes are recommended herein for the use of an FID. For definitions of gas chromatography and its various terms see recommended Practice E355.
1.5 For general information concerning the principles, construction, and operation of an FID, see Refs (1, 2, 3, 4).
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 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 specific safety information, see Section 5.
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Designation: E594 − 96 (Reapproved 2011)
Standard Practice for
Testing Flame Ionization Detectors Used in Gas or
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Supercritical Fluid Chromatography
This standard is issued under the fixed designation E594; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
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2.1 ASTM Standards:
1.1 This practice covers the testing of the performance of a
E260Practice for Packed Column Gas Chromatography
flame ionization detector (FID) used as the detection compo-
E355PracticeforGasChromatographyTermsandRelation-
nent of a gas or supercritical fluid (SF) chromatographic
ships
system.
2.2 CGA Standards:
1.2 This recommended practice is directly applicable to an
CGAP-1 Safe Handling of Compressed Gases in Contain-
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FID that employs a hydrogen-air or hydrogen-oxygen flame
ers
burner and a dc biased electrode system.
CGAG-5.4 Standard for Hydrogen Piping Systems at
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Consumer Locations
1.3 This recommended practice covers the performance of
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CGAP-9The Inert Gases: Argon, Nitrogen and Helium
the detector itself, independently of the chromatographic
CGAV-7Standard Method of Determining Cylinder Valve
column, the column-to-detector interface (if any), and other
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Outlet Connections for Industrial Gas Mixtures
systemcomponents,intermsthattheanalystcanusetopredict
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CGAP-12Safe Handling of Cryogenic Liquids
overall system performance when the detector is made part of
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HB-3Handbook of Compressed Gases
a complete chromatographic system.
3. Terminology
1.4 For general gas chromatographic procedures, Practice
3.1 Definitions:
E260 should be followed except where specific changes are
3.1.1 drift—the average slope of the baseline envelope
recommended herein for the use of an FID. For definitions of
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expressed in amperes per hour as measured over ⁄2 h.
gas chromatography and its various terms see recommended
Practice E355.
3.1.2 noise (short-term)—the amplitude expressed in am-
peres of the baseline envelope that includes all random
1.5 For general information concerning the principles,
variations of the detector signal of a frequency on the order of
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construction, and operation of an FID, see Refs (1, 2, 3, 4).
1 or more cycles per minute (see Fig. 1).
1.6 The values stated in SI units are to be regarded as 3.1.2.1 Discussion—Short-term noise corresponds to the
observed noise only. The actual noise of the system may be
standard. No other units of measurement are included in this
standard. larger or smaller than the observed value, depending upon the
method of data collection or signal monitoring from the
1.7 This standard does not purport to address all of the
detector, since observed noise is a function of the frequency,
safety concerns, if any, associated with its use. It is the
speed of response, and the bandwidth of the electronic circuit
responsibility of the user of this standard to establish appro-
measuring the detector signal.
priate safety and health practices and determine the applica-
3.1.3 other noise—Fluctuations of the baseline envelope of
bility of regulatory limitations prior to use. For specific safety
a frequency less than 1 cycle per minute can occur in
information, see Section 5.
chromatographic systems.
3.1.4 Discussion—The amplitude of these fluctuations may
actually exceed the short-term noise. Such fluctuations are
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This practice is under the jurisdiction ofASTM Committee E13 on Molecular
Spectroscopy and Separation Science and is the direct responsibility of Subcom-
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mittee E13.19 on Separation Science. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2011. Published December 2011. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1977. The last previous edition approved in 2006 as E594–96(2011). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/E0594-96R11. the ASTM website.
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The boldface numbers in parentheses refer to the list of references appended to Available from Compressed Gas Association (CGA), 4221 Walney Rd., 5th
this recommended practice. Floor, Chantilly, VA 20151-2923, http://www.cganet.com.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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E594 − 96 (2011)
FIG. 1 Example of the FID Noise Level and Drift Measurement
difficult to characterize and are not typically to be expected. responsibility of every laboratory. The CGA, a member group
Theyareusuallycausedbyotherchromatographiccomponents of sp
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