ASTM_E_2977_-_15.pdf

Designation:E297715Standard Practice forMeasuring and Reporting Performance of Fourier-TransformNuclear Magnetic Resonance(FT-NMR)Spectrometers forLiquid Samples1This standard is issued under the fixed designation E2977;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This practice covers procedures for measuring andreporting the performance of Fourier-transform nuclear mag-netic resonance spectrometers(FT-NMRs)using liquidsamples.1.2 This practice is not directly applicable to FT-NMRspectrometers outfitted to measure gaseous,anisotropicallystructured liquid,semi-solid,or solid samples;those set up towork with flowing sample streams;or those used to makehyperpolarization measurements.1.3 This practice was expressly developed for FT-NMRspectrometers operating with proton resonance frequenciesbetween 200 and 1200 MHz.1.4 This practice is not directly applicable to continuouswave(scanning)NMR spectrometers.1.5 This practice is not directly applicable to instrumentsusing single-sideband detection.1.6 UnitsThe values stated in SI units are to be regardedas the standard.No other units of measurement are included inthis standard.1.7 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2E131 Terminology Relating to Molecular SpectroscopyE386 Practice for Data Presentation Relating to High-Resolution Nuclear Magnetic Resonance(NMR)Spec-troscopy2.2 ISO Standard:3ISO Guide 31 Reference MaterialsContents of Certificatesand Labels3.Terminology3.1 DefinitionsFor definitions of terms used in thispractice,refer to Terminology E131,Practice E386,and Refs(1-4).4Chemical shifts are usually given in the dimensionlessquantity,commonly expressed in parts per million.For agiven nucleus,the chemical shift scale is relative and iscommonly pegged to the resonance of an agreed upon refer-ence material as described by Eq 1.sample5sample2 reference!reference(1)3.1.1 Frequencies are given in Hertz.Because the numeratoris very small compared with the denominator,it is usuallyconvenient to express in parts per million.3.1.2 As the location of a resonance is determined in part bythe ratio of the magnetic field to the radio frequency at whichit is observed,chemical shifts and spectral regions are oftendesignated as lower frequency(increased shielding)or higherfrequency(decreased shielding)relative to a reference point.Defined in this manner,chemical shifts are independent ofeither the magnetic field or the radio frequency used.Couplingconstants,which are independent of the magnetic field or radiofrequency used,are expressed in Hertz.3.1.3 nuclear magnetic resonance(NMR)tube camber,nmaximum total deflection of any part of the outer wall ofthe tube held at the ends and rotated 360;a measure of thebow in the tube.3.1.4 NMR tube concentricity,nmaximum variation inwall thickness of the tube;a measure of how centered the tubeinside diameter is relative to the tube outer diameter.1This test method is under the jurisdiction of ASTM Committee E13 onMolecular Spectroscopy and Separation Science and is the direct responsibility ofSubcommittee E13.15 on Analytical Data.Current edition approved May 1,2015.Published May 2015.Originallyapproved in 2014.Last previous edition approved in 2014 as E297714.DOI:10.1520/E2977-15.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute(ANSI),25 W.43rd St.,4th Floor,New York,NY 10036,http:/www.ansi.org.4The boldface numbers in parentheses refer to the list of references at the end ofthis standard.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 4.Significance and Use4.1 This practice permits an analyst to compare the perfor-mance of an NMR spectrometer for a particular test on anygiven day with the instruments prior performance for that test.The practice can also provide sufficient quantitative perfor-mance information for problem diagnosis and solving.Ifcomplete information about how a test is carried out is suppliedand sufficient replicates are collected to substantiate statisticalrelevance,the tests in this practice can be used to establish thesetting and meeting of relevant performance specifications.This practice is not necessarily meant for the comparison ofdifferent instruments with each other,even if the inst