1、Designation: E 475 00 (Reapproved 2005)Standard Test Method forAssay of Di-tert-Butyl Peroxide Using Gas Chromatography1This standard is issued under the fixed designation E 475; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the assay of di-tert-butylperoxide using gas chromatography. It is applicable to com-
3、mercial di-tert-butyl peroxide which may contain smallamounts of isobutylene, tert-butanol, tert-butyl hydroperoxide,triisobutylenes, and water as impurities.1.2 Review the current appropriate Material Safety DataSheets (MSDS) for detailed information concerning toxicity,first aid procedures, and sa
4、fety precautions.1.3 The values stated in 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
5、to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in Section 9.2. Referenced Documents2.1 ASTM Standards:2E 203 Test Method for Water Using Volumetric Karl FischerTitration3. Terminology
6、3.1 Definitions:3.1.1 active oxygenthe oxidizing power present in organicperoxides expressed as oxygen (equivalent weight = 8.00).4. Summary of Test Method4.1 A sample is diluted in dodecane and injected into a gaschromatograph containing a wide-bore capillary column with anonpolar stationary phase.
7、 A temperature program is used toseparate di-tert-butyl peroxide from impurities using helium asa carrier gas. The flame ionization detector response, propor-tional to component concentration, is recorded and the peakareas are measured. The concentration of di-tert-butyl peroxideis determined by are
8、a normalization after correcting for thearea of the solvent peak. The assay of di-tert-butyl peroxide iscorrected for water, which is determined using a separate KarlFischer titration since water is not detected using flameionization detection. The area percent of di-tert-butyl peroxideis assumed to
9、 be equal to weight percent.5. Significance and Use5.1 Di-tert-butyl peroxide is widely used as a catalyst andreaction initiator. Knowledge of the peroxide content is impor-tant in such applications. This test method provides a proce-dure for determining the active peroxide content of commercialdi-t
10、ert-butyl peroxide.6. Interferences6.1 Interferences will be encountered if other componentsare present in the sample that have the same retention time asdi-tert-butyl peroxide.7. Apparatus7.1 InstrumentationGas chromatograph, capable of col-umn oven temperature programming from 40 to 160C at a rate
11、of 10C/min and from 160 to 240C at a rate of 35C/min.7.2 Injection SystemGlass-lined sample injection port,maintained at 150C.7.3 Sample IntroductionMicroliter syringes or automaticsyringe injectors, capable of delivering 0.5 L of a liquidsample, have been used successfully.7.4 DetectionFlame ioniza
12、tion detector, maintained at250C.7.5 Data Acquisition SystemElectronic data acquisitionand area integration capabilities are recommended.7.6 Chromatographic Column30 m wide-bore capillarycolumn (0.53 mm inside diameter) with a 5.0 m dimethylpol-ysiloxane stationary phase.38. Reagents and Materials8.
13、1 Carrier Gas (Helium), chromatographic grade.8.2 Hydrogen, chromatographic grade.1This test method is under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and is the direct responsibility of SubcommitteeE15.02 on Product Standards.Current edition approved Oct. 1, 2005.
14、Published November 2005. Originallyapproved in 1973. Last previous edition approved in 2000 as E 475 00.2For 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 standard
15、s Document Summary page onthe ASTM website.3AJ di-tert-butyl peroxide; gas chromatog-raphy; peroxides4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: E15-1044.TABLE 1 Operating Conditions Required to Give the DesiredSeparationDe
16、tector flame ionization (FID)Temperatures, CInjection port 150Detector 250Column temperature programInitial temperature, C 40Initial time, min 3Program rate, C/min 10Temperature 2, C 160Time 2, min 2Program rate, C/min 35Final temperature, C 240Final time, min 2Carrier gas heliumFlow rate, mL/min 10
17、.0Injection volume, L 0.5E 475 00 (2005)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and th
18、e riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision o
19、f this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
20、make your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).FIG. 1 Typical ChromatogramFIG. 2 Typical Chromatogram (Expanded View)E 475 00 (2005)3
