ASTM E594-96(2006)
(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’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, Refs. (5,6) 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 E 260 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 E 355.
1.5 For general information concerning the principles, construction, and operation of an FID, see Refs (1, 2, 3, 4).
1.6 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 .
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Designation:E594–96(Reapproved 2006)
Standard Practice for
Testing Flame Ionization Detectors Used in Gas or
1
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 E355 Practice for Gas Chromatography Terms and Rela-
tionships
1.1 This practice covers the testing of the performance of a
2.2 CGA Standards:
flame ionization detector (FID) used as the detection compo-
CGAP-1 Safe Handling of Compressed Gases in Contain-
nent of a gas or supercritical fluid (SF) chromatographic
4
ers
system.
CGAG-5.4 Standard for Hydrogen Piping Systems at
1.2 This recommended practice is directly applicable to an
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Consumer Locations
FID that employs a hydrogen-air or hydrogen-oxygen flame
4
CGAP-9 The Inert Gases: Argon, Nitrogen and Helium
burner and a dc biased electrode system.
CGAV-7 Standard Method of Determining CylinderValve
1.3 This recommended practice covers the performance of
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Outlet Connections for Industrial Gas Mixtures
the detector itself, independently of the chromatographic col-
4
CGAP-12 Safe Handling of Cryogenic Liquids
umn, the column-to-detector interface (if any), and other
4
HB-3 Handbook of Compressed Gases
systemcomponents,intermsthattheanalystcanusetopredict
overall system performance when the detector is made part of
3. Terminology
a complete chromatographic system.
3.1 Definitions:
1.4 For general gas chromatographic procedures, Practice
3.1.1 drift—the average slope of the baseline envelope
E260 should be followed except where specific changes are
1
expressed in amperes per hour as measured over ⁄2 h.
recommended herein for the use of an FID. For definitions of
3.1.2 noise (short-term)—the amplitude expressed in am-
gas chromatography and its various terms see Recommended
peres of the baseline envelope that includes all random
Practice E355.
variations of the detector signal of a frequency on the order of
1.5 For general information concerning the principles, con-
2 1 or more cycles per minute (see Fig. 1).
struction, and operation of an FID, see Refs (1, 2, 3, 4).
3.1.2.1 Discussion— Short-term noise corresponds to the
1.6 This standard does not purport to address all of the
observed noise only. The actual noise of the system may be
safety concerns, if any, associated with its use. It is the
larger or smaller than the observed value, depending upon the
responsibility of the user of this standard to establish appro-
method of data collection or signal monitoring from the
priate safety and health practices and determine the applica-
detector, since observed noise is a function of the frequency,
bility of regulatory limitations prior to use. For specific safety
speed of response, and the bandwidth of the electronic circuit
information, see Section 5.
measuring the detector signal.
2. Referenced Documents 3.1.3 other noise—Fluctuations of the baseline envelope of
3 a frequency less than 1 cycle per minute can occur in
2.1 ASTM Standards:
chromatographic systems.
E260 Practice for Packed Column Gas Chromatography
3.1.4 Discussion—The amplitude of these fluctuations may
actually exceed the short-term noise. Such fluctuations are
1
This practice is under the jurisdiction ofASTM Committee E13 on Molecular
difficult to characterize and are not typically to be expected.
Spectroscopy and is the direct responsibility of Subcommittee E13.19 on Chroma-
Theyareusuallycausedbyotherchromatographiccomponents
tography.
such as the column, system contaminants, and flow variations.
Current edition approved March 1, 2006. Published March 2006. Originally
approved in 1977. The last previous edition approved in 2001 as E594–96(2001).
These other noise contributions are not derived from the
DOI: 10.1520/E0594-96R06.
detector itself and are difficult to quantitate in a general
2
The boldface numbers in parentheses refer to the list of references appended to
this recommended practice.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
4
Standards volume information, refer to the standard’s Document Summary page on Available from Compressed Gas Association (CGA), 1725 Jefferson Davis
the ASTM website. Hwy., Suite 1004, Arlington, VA 22202-4102.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E594–96 (2006)
FIG. 1 Example of the FID Noise Level and Drift Measurement.
manner.Itis,however,importantforthepractic
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