Standard Practice for Measuring and Reporting Performance of Fourier-Transform Nuclear Magnetic Resonance (FT-NMR) Spectrometers for Liquid Samples

SIGNIFICANCE AND USE
4.1 This practice permits an analyst to compare the performance of an NMR spectrometer for a particular test on any given day with the instrument's prior performance for that test. The practice can also provide sufficient quantitative performance information for problem diagnosis and solving. If complete information about how a test is carried out is supplied and sufficient replicates are collected to substantiate statistical relevance, the tests in this practice can be used to establish the setting and meeting of relevant performance specifications. This practice is not necessarily meant for the comparison of different instruments with each other, even if the instruments are of the same type and model. This practice is not meant for the comparison of the performance of different instruments operated under conditions differing from those specified for a particular test.
SCOPE
1.1 This practice covers procedures for measuring and reporting the performance of Fourier-transform nuclear magnetic resonance spectrometers (FT-NMRs) using liquid samples.  
1.2 This practice is not directly applicable to FT-NMR spectrometers outfitted to measure gaseous, anisotropically structured liquid, semi-solid, or solid samples; those set up to work with flowing sample streams; or those used to make hyperpolarization measurements.  
1.3 This practice was expressly developed for FT-NMR spectrometers operating with proton resonance frequencies between 200 and 1200 MHz.  
1.4 This practice is not directly applicable to continuous wave (scanning) NMR spectrometers.  
1.5 This practice is not directly applicable to instruments using single-sideband detection.  
1.6 Units—The values stated in SI units are to be regarded as the 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.

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Status
Historical
Publication Date
31-Jul-2014
Current Stage
Ref Project

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ASTM E2977-14 - Standard Practice for Measuring and Reporting Performance of Fourier-Transform Nuclear Magnetic Resonance (FT-NMR) Spectrometers for Liquid Samples
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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: E2977 − 14
StandardPractice for
Measuring and Reporting Performance of Fourier-Transform
Nuclear Magnetic Resonance (FT-NMR) Spectrometers for
1
Liquid Samples
This standard is issued under the fixed designation E2977; 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 Resolution Nuclear Magnetic Resonance (NMR) Spec-
troscopy
1.1 This practice covers procedures for measuring and
3
reporting the performance of Fourier-transform nuclear mag- 2.2 ISO Standard:
netic resonance spectrometers (FT-NMRs) using liquid ISOGuide31ReferenceMaterials—ContentsofCertificates
samples. and Labels
1.2 This practice is not directly applicable to FT-NMR
3. Terminology
spectrometers outfitted to measure gaseous, anisotropically
structured liquid, semi-solid, or solid samples; those set up to
3.1 Definitions—For definitions of terms used in this
work with flowing sample streams; or those used to make practice, refer to Terminology E131, Practice E386, and Refs
4
hyperpolarization measurements.
(1-4). Chemical shifts are usually given in the dimensionless
quantity, δ, commonly expressed in parts per million. For a
1.3 This practice was expressly developed for FT-NMR
given nucleus, the chemical shift scale is relative and is
spectrometers operating with proton resonance frequencies
commonly pegged to the resonance of an agreed upon refer-
between 200 and 1200 MHz.
ence material as described by Eq 1.
1.4 This practice is not directly applicable to continuous
δ 5 ~ν 2 ν ! ÷ν (1)
sample sample reference reference
wave (scanning) NMR spectrometers.
3.1.1 FrequenciesaregiveninHertz.Becausethenumerator
1.5 This practice is not directly applicable to instruments
is very small compared with the denominator, it is usually
using single-sideband detection.
convenient to express δ in parts per million.
1.6 Units—The values stated in SI units are to be regarded
3.1.2 Asthelocationofaresonanceisdeterminedinpartby
as the standard. No other units of measurement are included in
the ratio of the magnetic field to the radio frequency at which
this standard.
it is observed, chemical shifts and spectral regions are often
1.7 This standard does not purport to address all of the
designated as lower frequency (increased shielding) or higher
safety concerns, if any, associated with its use. It is the
frequency (decreased shielding) relative to a reference point.
responsibility of the user of this standard to establish appro-
Defined in this manner, chemical shifts are independent of
priate safety and health practices and determine the applica-
either the magnetic field or the radio frequency used. Coupling
bility of regulatory limitations prior to use.
constants,whichareindependentofthemagneticfieldorradio
frequency used, are expressed in Hertz.
2. Referenced Documents
3.1.3 nuclear magnetic resonance (NMR) tube camber,
2
2.1 ASTM Standards: n—maximum total deflection of any part of the outer wall of
E131Terminology Relating to Molecular Spectroscopy the tube held at the ends and rotated 360°; a measure of the
E386Practice for Data Presentation Relating to High- bow in the tube.
3.1.4 NMR tube concentricity, n—maximum variation in
wall thickness of the tube; a measure of how centered the tube
1
This test method is under the jurisdiction of ASTM Committee E13 on
inside diameter is relative to the tube outer diameter.
Molecular Spectroscopy and Separation Science and is the direct responsibility of
Subcommittee E13.15 on Analytical Data.
Current edition approved Aug. 1, 2014. Published September 2014. DOI:
10.1520/E2977-14.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 4th Floor, New York, NY 10036, http://www.ansi.org.
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Standards volume information, refer to the standard’s Document Summary page on Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
the ASTM website. this standard.
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E2977 − 14
4. Significance and Use resonances of impurities observed in the spectrum of the
standard sample should not interfere with the resonances of
4.1 This practice permits an analyst to compare the perfor-
interest in the standard sample. This usually means that the
mance of an NMR spectrometer for a particular test on any
impurity peaks shall not appear within the region of the
givendaywitht
...

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