Name: ASTM E685-93(2013) - Standard Practice for Testing Fixed-Wavelength Photometric Detectors Used in Liquid Chromatography
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Abstract

Standard Practice for Testing Fixed-Wavelength Photometric Detectors Used in Liquid Chromatography

General Information

Status

Historical

Publication Date

31-Dec-2012

ICS

17.180.30 - Optical measuring instruments

71.040.50 - Physicochemical methods of analysis

Technical Committee

E13 - Molecular Spectroscopy and Separation Science

Drafting Committee

E13.19 - Separation Science

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ASTM E685-93(2013) - Standard Practice for Testing Fixed-Wavelength Photometric Detectors Used in Liquid Chromatography

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ASTM E685-93(2013) - Standard ...

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E685 − 93 (Reapproved 2013)
Standard Practice for
Testing Fixed-Wavelength Photometric Detectors Used in
1
Liquid Chromatography
This standard is issued under the ﬁxed designation E685; 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 3. Terminology
1.1 This practice is intended to serve as a guide for the 3.1 Deﬁnitions:
testingoftheperformanceofaphotometricdetector(PD)used 3.1.1 absorbance calibration, n—the procedure that veriﬁes
as the detection component of a liquid-chromatographic (LC) that the absorbance scale is correct within 65%.
systemoperatingatoneormoreﬁxedwavelengthsintherange
3.1.2 drift, n—the average slope of the noise envelope
210to800nm.Measurementsaremadeat254nm,ifpossible,
expressed in absorbance units per hour (AU/h) as measured
and are optional at other wavelengths.
over a period of 1 h.
1.2 This practice is intended to describe the performance of
3.1.3 dynamic, n—under conditions of a ﬂow rate of 1.0
thedetectorbothindependentlyofthechromatographicsystem
mL/min.
(static conditions) and with ﬂowing solvent (dynamic condi-
3.1.4 linear range, n— of a PD, the range of concentrations
tions).
of a test substance in a mobile phase over which the response
1.3 For general liquid chromatographic procedures, consult ofthedetectorisconstanttowithin5%asdeterminedfromthe
2
Refs (1-9). linearity plot speciﬁed below and illustrated in Fig. 1. The
linear range should be expressed as the ratio of the highest
1.4 For general information concerning the principles,
concentration to the minimum detectable concentration or the
construction, operation, and evaluation of liquid-
lowest linear concentration, whichever is greatest.
chromatography detectors, see Refs (10 and 11) in addition to
3.1.5 long-term noise, n—the maximum amplitude in AU
the sections devoted to detectors in Refs (1-7).
for all random variations of the detector signal of frequencies
1.5 This standard does not purport to address all of the
between6and60cyclesperhour(0.1and1.0cyclespermin).
safety problems, if any, associated with its use. It is the
3.1.5.1 Discussion—Itrepresentsnoisethatcanbemistaken
responsibility of the user of this standard to establish appro-
for a late-eluting peak. This noise corresponds to the observed
priate safety and health practices and determine the applica-
noise only and may not always be present.
bility of regulatory limitations prior to use.
3.1.6 minimum detectability, n—of a PD, that concentration
ofaspeciﬁcsoluteinaspeciﬁcsolventthatresultsinadetector
2. Referenced Documents
response corresponding to twice the static short-term noise.
3
2.1 ASTM Standards:
3.1.7 response time (speed of output), n—the detector, the
E275PracticeforDescribingandMeasuringPerformanceof
timerequiredforthedetectoroutputtochangefrom10to90%
Ultraviolet and Visible Spectrophotometers
of the new equilibrium value when the composition of the
E682Practice for Liquid Chromatography Terms and Rela-
mobilephaseischangedinastepwisemanner,withinthelinear
tionships
range of the detector.
3.1.7.1 Discussion—Because the detector volume is very
small and the transport rate is not diffusion dependent, the
1
This practice is under the jurisdiction ofASTM Committee E13 on Molecular
response time is generally fast enough to be unimportant. It is
Spectroscopy and Separation Science and is the direct responsibility of Subcom-
generally comparable to the response time of the recorder and
mittee E13.19 on Separation Science.
Current edition approved Jan. 1, 2013. Published January 13. Originally
dependent on the response time of the detector electrometer
approved in 1979. Last previous edition approved in 2005 as E685–93(2005).
and on the recorder ampliﬁer. Factors that affect the observed
DOI: 10.1520/E0685-93R13.
response time include the true detector response time, elec-
2
Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
tronic ﬁltering, and system band-broadening.
this practice.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.1.8 short-term noise, n—the maximum amplitude, peak to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
peak, inAU for all random variations of the detector signal of
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. a frequency greater than one cycle per minute.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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E685 − 93 (2013)
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4.1 This practice permits an analyst to compare the performance of an instrument to the manufacturer's supplied performance specifications and to verify its suitability for continued routine use. It also provides generation of calibration monitoring data on a periodic basis, forming a base from which any changes in the performance of the instrument will be evident.
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4.1 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 practice that a complete set of detector specifications should be obtained under the same operating conditions. It should also be noted that to completely specify a detector’s capability, its performance should be measured at several sets of conditions within the useful range of the detector. The terms and tests described in this practice are sufficiently general that they may be used regardless of the ultimate operating parameters.
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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.
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3.1 Although it is possible to observe and measure each of several characteristics of a detector under different and unique conditions, it is the intent of this practice that a complete set of detector test results should be obtained under the same operating conditions. It should also be noted that to specify completely a detector's capability, its performance should be measured at several sets of conditions within the useful range of the detector.
3.2 The objective of this practice is to test the detector under specified conditions and in a configuration without an LC column. This is a separation independent test. In certain circumstances it might also be necessary to test the detector in the separation mode with an LC column in the system, and the appropriate concerns are also mentioned. The terms and tests described in this practice are sufficiently general so that they may be adapted for use at whatever conditions may be chosen for other reasons.
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1.1 This practice covers tests used to evaluate the performance and to list certain descriptive specifications of a refractive index (RI) detector used as the detection component of a liquid chromatographic (LC) system.
1.2 This practice is intended to describe the performance of the detector both independent of the chromatographic system (static conditions, without flowing solvent) and with flowing solvent (dynamic conditions).
1.3 The values stated in SI units are to be regarded as the standard.
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.