ASTM E932-89(2013)
(Practice)Standard Practice for Describing and Measuring Performance of Dispersive Infrared Spectrometers
Standard Practice for Describing and Measuring Performance of Dispersive Infrared Spectrometers
SIGNIFICANCE AND USE
4.1 This practice is intended for all infrared spectroscopists who are using dispersive instruments for qualitative or quantitative areas of analysis.
4.2 The purpose of this practice is to set forth performance guidelines for testing instruments used in developing an analytical method. These guidelines can be used to compare an instrument in a specific application with the instrument(s) used in developing the method.
4.3 An infrared procedure must include a description of the instrumentation and of the performance needed to duplicate the precision and accuracy of the method.
SCOPE
1.1 This practice covers the necessary information to qualify dispersive infrared instruments for specific analytical applications, and especially for methods developed by ASTM International.
1.2 This practice is not to be used as a rigorous test of performance of instrumentation.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety problems, 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.
General Information
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: E932 − 89 (Reapproved 2013)
Standard Practice for
Describing and Measuring Performance of Dispersive
Infrared Spectrometers
This standard is issued under the fixed designation E932; 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 Standard Definitions.
1.1 This practice covers the necessary information to
4. Significance and Use
qualify dispersive infrared instruments for specific analytical
4.1 This practice is intended for all infrared spectroscopists
applications, and especially for methods developed by ASTM
who are using dispersive instruments for qualitative or quan-
International.
titative areas of analysis.
1.2 This practice is not to be used as a rigorous test of
4.2 The purpose of this practice is to set forth performance
performance of instrumentation.
guidelines for testing instruments used in developing an
1.3 The values stated in SI units are to be regarded as
analyticalmethod.Theseguidelinescanbeusedtocomparean
standard. No other units of measurement are included in this
instrumentinaspecificapplicationwiththeinstrument(s)used
standard.
in developing the method.
1.4 This standard does not purport to address all of the
4.3 An infrared procedure must include a description of the
safety problems, if any, associated with its use. It is the
instrumentationandoftheperformanceneededtoduplicatethe
responsibility of the user of this standard to establish appro-
precision and accuracy of the method.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Apparatus
5.1 For the purposes of this practice, dispersive instruments
2. Referenced Documents
include those employing prisms, gratings, or filters to separate
2.1 ASTM Standards:
infrared radiation into its component wavelengths.
E131Terminology Relating to Molecular Spectroscopy
5.2 For each new method, describe the apparatus and
E168Practices for General Techniques of Infrared Quanti-
instrumentation both physically and mechanically, and also in
tative Analysis (Withdrawn 2015)
terms of performance as taught in this practice. That is, the
E387TestMethodforEstimatingStrayRadiantPowerRatio
description should give numerical values showing the fre-
of Dispersive Spectrophotometers by the Opaque Filter
quency accuracy and the frequency and the photometric
Method
precision. State the spectral slit width maximum or slit width
E1252Practice for General Techniques for Obtaining Infra-
programifoneisused.Wherepossible,statethemaximumand
red Spectra for Qualitative Analysis
minimum resolution if those data are a part of the instrument
3. Terminology display. Show typical component spectra as produced by the
instrument to establish the needed resolution.
3.1 Definitions and Symbols—For definitions of terms and
symbols,refertoTerminologyE131and Compilation of ASTM 5.3 If a computer program is used, describe the program.
Includetheprogramminglanguageandavailability,orwhether
the program is proprietary to a manufacturer.
This practice is under the jurisdiction ofASTM Committee E13 on Molecular
Spectroscopy and Separation Science and is the direct responsibility of Subcom-
6. Reference to this Practice in Standards
mittee E13.03 on Infrared and Near Infrared Spectroscopy.
Current edition approved Jan. 1, 2013. Published January 2013. Originally 6.1 Reference to this practice should be included in all
approved in 1989. Last previous edition approved in 2007 as E932–89(2007).
ASTM infrared methods. The reference should appear in the
DOI: 10.1520/E0932-89R13.
section on apparatus where the particular spectrometer is
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
described.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3 4
The last approved version of this historical standard is referenced on Available fromASTM International Headquarters, 100 Barr Harbor Drive, PO
www.astm.org. Box C700, West Conshohocken, PA 19428.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E932 − 89 (2013)
7. Parameters in Spectroscopy 8.5 In the case of computerized dispersive instruments, any
spectrum printed from a computer file must be obtained as
7.1 Dispersive infrared spectrometers have a source of
prescribed by the manufacturer and should be identical to the
quasi-monochromatic radiation together with a photometer for
original data.
measuring relative radiant power. Accurate spectrometry in-
volvesalargenumberofinterrelatedfactorsthatdeterminethe
PRECISION AND ACCURACY
quality of the radiant power passing through a sample and the
sensitivity and linearity with which this radiant power can be
9. Definitions
measured. Assuming proper instrumentation and its use, the
9.1 wavenumber precision—ameasureofthecapabilityofa
instrumental factors responsible for inaccuracies in spectrom-
spectrometer to return to the same spectral position as mea-
etry are resolution, linearity (Practices E168), stray radiant
sured by a well-defined absorption or emission band when the
power (Test Method E387), and cell constants (Practice
instrumentisresetorrescanned.Theindexusedinthispractice
E1252). Rigorous measurement of these factors is beyond the
is the standard deviation.
scope of this practice, and a more practical approach is
9.2 wavenumber accuracy—the deviation of the average
described for the accessible factors.
wavenumber reading of an absorption band or emission band
from the known wavenumber of that band.
8. Instrument Operation
8.1 The analyst selects the proper instrumental operating
10. Nature of Test
conditions in order to get satisfactory performance (1-3).
10.1 For the purpose of calibration, most methods employ
Because instrument design varies, the manufacturer’s recom-
pure compounds and known mixtures at specified analytical
mendations are usually best. A record of operating conditions
wavenumbers. The wavenumbers are either read from a dial,
should be kept so that data can be duplicated by future users.
optical display, chart paper, or a computer file.
8.2 Inadditiontooperatingconditions,thefollowingshould
11. Reference Wavenumbers in the Infrared Region (2)
be checked and recorded:
8.2.1 Ambient temperature,
11.1 The recommended wavenumber calibration points are
8.2.2 Pen response time,
the absorption maxima of a standard (98.4/0.8/0.8 by weight)
8.2.3 Scanning speed,
indene/camphor/cyclohexanonemixturelistedinTable1.Suit-
able path lengths are 0.2 mm for the range from 3800 to 1580
NOTE1—Insomeinstrumentsthesefunctionsareintegratedinthescan
−1
cm and0.03mmforthewavenumberrangefrom1600to600
modes.
-1
cm . A mixture containing equal parts by weight of indene,
8.2.4 Noise level, and
camphor,andcyclohexanone(1/1/1byweight)atapathlength
8.2.5 Mechanical repeatability.
8.3 Each of the above factors is important in the measure-
TABLE 1 Indene-Camphor-Cyclohexanone (98.4/0.8/0.8) Mixture—
ment of analytical wavenumber and photometric data.There is
Recommended Calibration Bands
usually some lag between the recorded reading and the correct
NOTE 1—Table 1 and Table 2 contain wavenumber values for bands in
reading. Proper selection of operating conditions and good,
Fig. 1.
reproducible, sample handling techniques minimize these ef-
Band Wavenumber, Band Wavenumber,
fects or make the effects repeatable. For example:
−1 −1
No. cm No. cm
8.3.1 Variation in temperature of the monochromator or
1 3927.2 ± 1.0 44α 1741.9
sample may cause changes in wavenumber precision and
2 3901.6 44β 1713.4
3 3798.9 47 1661.8
accuracy.
5 3660.6 ± 1.0 48 1609.8
8.3.2 Scanningtoofastwilldisplacetheapparentwavenum-
8 3297.8 ± 1.0 49 1587.5
ber towards the direction scanned and will decrease the peak
9 3139.5 51 1553.2
10 3110.2 53 1457.3 ± 1.0
absorbance reading for each band.
12 3025.4 54 1393.5
15 2887.6 55 1361.1
NOTE 2—Some instruments provide for automatic monitoring and
17 2770.9 57 1312.4
correction of this effect.
19 2673.3 58 1288.0
8.4 Mechanical repeatability of the monochromator and 20 2622.3 60 1226.2
21 2598.4 ± 1.0 61 1205.1
recording system as well as positioning of chart paper are
23 2525.5 62 1166.1
important in wavenumber measurement.
28 2305.1 64 1122.4
8.4.1 Chart paper should be checked for uniformity of the 29 2271.4 66 1067.7 ± 1.0
30 2258.7 67 1018.5
printed scale length as received and rechecked at time of use,
33 2172.8 69 947.2
particularly if the paper has been subjected to pronounced
34 2135.8 ± 1.0 70 942.4
35 2113.2 71 914.7
humiditychanges.Instructionsonobtainingpropermechanical
36 2090.2 72 861.3
repeatability may be given in the manufacturer’s literature.
39 1943.1 73 830.5
40 1915.3 74 765.3
41 1885.1 76 718.1
42 1856.9 77 692.6 ± 1.0
The boldface numbers in parentheses refer to a list of references at the end of 44 1797.7 ± 1.0
this standard.
E932 − 89 (2013)
−1
of 0.1 mm may be used for the range from 600 to 300 cm . 13.2 The preferred manner of expressing resolution is in
See Table 2 and Fig. 1. terms of spectral band width, but methods of measuring this
quantity in all spectral regions are not available.
11.2 Polystyrene is also a convenient calibration standard
−1 13.2.1 Spectral band width is not constant throughout the
forthewavenumberrangefrom4000to400cm .Polystyrene
spectrum and theref
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