ASTM E2106-2000(2011) Standard Practice for General Techniques of Liquid Chromatography-Infrared (LC IR) and Size Exclusion Chromatography-Infrared (SEC IR) Analyses《红外线液色谱和红外线大小排除.pdf
《ASTM E2106-2000(2011) Standard Practice for General Techniques of Liquid Chromatography-Infrared (LC IR) and Size Exclusion Chromatography-Infrared (SEC IR) Analyses《红外线液色谱和红外线大小排除.pdf》由会员分享,可在线阅读,更多相关《ASTM E2106-2000(2011) Standard Practice for General Techniques of Liquid Chromatography-Infrared (LC IR) and Size Exclusion Chromatography-Infrared (SEC IR) Analyses《红外线液色谱和红外线大小排除.pdf(7页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: E2106 00 (Reapproved 2011)Standard Practice forGeneral Techniques of Liquid Chromatography-Infrared (LC/IR) and Size Exclusion Chromatography-Infrared (SEC/IR)Analyses1This standard is issued under the fixed designation E2106; the number immediately following the designation indicates t
2、he 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 techniques that are of gener
3、al use inqualitatively analyzing multicomponent samples by using acombination of liquid chromatography (LC) or size exclusionchromatography (SEC) with infrared (IR) spectrometric tech-niques. The sample mixture is separated into fractions by thechromatographic separation. These fractions are subsequ
4、entlyanalyzed by an IR spectroscopic method.1.2 Three different types of LC/IR techniques have beenused to analyze samples (1, 2).2These consist of eluenttrapping (see Practices E334), flowcell and direct deposition.These are presented in the order that they were first used.1.3 The values stated in
5、SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 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 healt
6、h practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3E131 Terminology Relating to Molecular SpectroscopyE168 Practices for General Techniques of Infrared Quanti-tative AnalysisE334 Practice for General Techniques of Infrared M
7、icro-analysisE1421 Practice for Describing and Measuring Performanceof Fourier Transform Mid-Infrared (FT-MIR) Spectrom-eters: Level Zero and Level One Tests3. Terminology3.1 DefinitionsFor definitions of terms and symbols, referto Terminology E131.3.2 Definitions of Terms Specific to This Standard:
8、3.2.1 hit quality index (HQI), nthe comparison of infraredspectroscopic data against a database of reference spectra ofknown compounds is often employed to assist in the determi-nation of the evolved gas chemical identity. Search algorithmsgenerate a listing of reference compounds from the databaset
9、hat are spectroscopically similar to the evolved gas spectrum.These reference compounds are ranked with regard to ameasurement of the comparative fit of the reference spectraldata to that of the spectrum of the evolved gas. This ranking isreferred to as the hit quality index (HQI).4. Significance an
10、d Use4.1 This practice provides general guidelines for the prac-tice of liquid chromatography or size exclusion chromatogra-phy coupled with infrared spectrometric detection and analysis(LC/IR, SEC/IR). This practice assumes that the chromatogra-phy involved is adequate to resolve a sample into disc
11、retefractions. It is not the intention of this practice to instruct theuser on how to perform liquid or size exclusion chromatogra-phy (LC or SEC).5. General LC/IR Techniques5.1 Three different LC/IR techniques have been used toanalyze samples. These consist of eluent trapping, flowcell anddirect de
12、position. These are presented in the order that theywere first developed. Infrared detection for any of thesetechniques can be provided by IR monochromators, IR filterspectrometers and Fourier transform infrared spectrometers(FT-IR). These detectors yield either single absorption band ortotal infrar
13、ed spectrum detection modes. Detection mode isdependent upon the type of IR detector employed and theacquisition time required by the LC or SEC experiment.1This practice is under the jurisdiction of ASTM Committee E13 on MolecularSpectroscopy and Separation Science and is the direct responsibility o
14、f Subcom-mittee E13.03 on Infrared and Near Infrared Spectroscopy.Current edition approved Nov. 1, 2011. Published December 2011. Originallyapproved in 2000. Last previous edition approved in 2006 as E2106 00 (2006).DOI: 10.1520/E2106-00R11.2The boldface numbers in parentheses refer to the list of r
15、eferences at the end ofthis standard.3For 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.1Copyright ASTM Internat
16、ional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.2 Eluent Trapping TechniquesEluent trapping tech-niques, such as stopped flow and fraction collection, are thesimple means for obtaining LC/IR data. In these techniques,the eluting sample is collected from t
17、he chromatograph indiscrete aliquots. These aliquots are then analyzed with theappropriate sampling accessory in an infrared spectrometer. Inutilizing such techniques, it is essential that a suitable LCdetector, such as refractive index or UV/VIS, be employed toallow definition of component elution.
18、 Since the analyte ofinterest is trapped physically, the spectrum can be recordedusing a long integration or scan coaddition time to improve thesignal-to-noise ratio (SNR). Generally, the stopped flow tech-nique requires the use of a flow cell and the IR spectrumacquired contains both analyte and mo
19、bile phase spectralfeatures. The fraction collection mode permits examination ofthe eluent as a solution of analyte and mobile phase or, withproper solvent removal, the analyte alone (provided that theanalyte is nonvolatile). As such, the fraction collection modewould require either a liquid cell fo
20、r solutions or a solidsubstrate, that is, KBr window for transmission, first surfacemirror for reflection-absorption or powdered KBr for diffusereflection measurements.5.3 Flowcell DetectionWith flowcell detection, the LCeluent is monitored continuously in the timeframe of thechromatography (real-ti
21、me) by the IR spectrometer with theuse of specially designed liquid cells (3-9). Liquid cells aredesigned to minimize dead volume and analyte mixing, toconserve chromatographic resolution, and achieve maximumoptical interaction of the eluent with the infrared radiation. Asthe effluent is a condensed
22、 phase, several cell types have beendevised to accommodate most experimental approaches for IRspectrometry, that is, transmission, reflection-absorption andattenuated total reflection (7). The flowcell technique typicallyyields submicrogram detection limits for most analytes (1).Typically, flowcells
23、 are mounted within the sample compart-ment of the spectrometer and use beam condensation optics todirect the IR beam into and out of the small volume of the cell.It is important to employ a mobile phase having low orpreferably no infrared absorptions in the analytically importantspectral regions fo
24、r the analytes of interest.As such, the choiceof mobile phase may constrain the liquid chromatographicseparation. Generally, this limits the chromatographic separa-tion to a normal phase type where nonpolar solvents likechloroform and carbon tetrachloride have sufficient solventstrength to elute com
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