1、Designation: D 5060 07Standard Test Method forDetermining Impurities in High-Purity Ethylbenzene by GasChromatography1This standard is issued under the fixed designation D 5060; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear 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. Scope*1.1 This test method describes the analysis of normallyoccurring impurities in, and the purity of, ethylbenzene b
3、y gaschromatography. Impurities determined include nonaromatichydrocarbons, benzene, toluene, xylenes, cumene, and dieth-ylbenzene isomers.1.2 This test method is applicable for impurities at concen-trations from 0.001 to 1.000 % and for ethylbenzene purities of99 % or higher. At this level, p-xylen
4、e may not be detected.1.3 In determining the performance of the test results usingthis method to applicable specifications, results shall berounded off in accordance with the rounding-off method ofPractice E29.1.4 This standard does not purport to address all of thesafety concerns, if any, associate
5、d 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. For a specifichazard statement, see Section 8.2. Referenced Documents2.1 ASTM Standards:2D 3437 Practice
6、 for Sampling and Handling Liquid CyclicProductsD 4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD 6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE29 Practice for Using Significant Digits in Test Data toDet
7、ermine Conformance with SpecificationsE 355 Practice for Gas Chromatography Terms and Rela-tionshipsE 1510 Practice for Installing Fused Silica Open TubularCapillary Columns in Gas Chromatographs2.2 Other Documents:OSHA Regulations, 29 CFR, paragraphs 1910.1000 and1910.120033. Summary of Test Method
8、3.1 A known amount of internal standard is added to thesample. A gas chromatograph equipped with a flame ionizationdetector and a polar fused silica capillary column is used forthe analysis. The impurities are measured relative to theinternal standard. Ethylbenzene purity is calculated by sub-tracti
9、ng the impurities found from 100.00 %.4. Significance and Use4.1 The test is suitable for setting specifications on ethyl-benzene and for use as an internal quality control tool whereethylbenzene is used in manufacturing processes. It may beused in development or research work involving ethylbenzene
10、.4.2 Purity is commonly reported by subtracting the deter-mined expected impurities from 100 %.Absolute purity cannotbe determined if unknown impurities are present.5. Interferences5.1 A key operational parameter for this method is theseparation of p-xylene from ethylbenzene. Care should betaken dur
11、ing calibration to ensure the separation of these twocomponents. If p-xylene is not separated from ethylbenzeneduring the calibration of the instrument, modify the columnflow rate slightly until separation is achieved.6. Apparatus6.1 Gas Chromatograph (GC)any GC built for capillarycolumn chromatogra
12、phy and equipped with a flame ionizationdetector (FID). The system shall have sufficient sensitivity,linearity, and range to obtain a minimum peak height responsefor 0.0010 wt% impurity of twice the height of the signalbackground noise, while not exceeding the full scale of either1This test method i
13、s under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.07 on Styrene, Ethylbenzene and C9 and C10 AtomaticHydrocarbons.Current edition approved Jan. 1, 2007. Published January 2007. Originallyapproved in 1990.
14、Last previous edition approved in 2006 as D 5060 06.2For 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.3Availabl
15、e from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshoho
16、cken, PA 19428-2959, United States.the detector or the electronic integration for the major compo-nents. It shall have a split injection system that will notdiscriminate over the boiling range of the samples analyzed.6.2 Chromatographic Column, fused silica capillary, 60 mlong, 0.32-mm inside diamet
17、er, internally coated to a 0.5-mthickness with a bonded (crosslinked) polyethylene glycol.Other columns may be used after it has been established thatsuch column is capable of separating all major impurities andthe internal standard from the ethylbenzene under operatingconditions appropriate for the
18、 column.6.3 Recorder, 1-mV,1sorless full scale response orelectronic integration with tangent capabilities (recom-mended).6.4 Microsyringe, 10-L.6.5 Microsyringe, 50-L.6.6 Volumetric Flask, 50-mL.7. Reagents and Materials7.1 Carrier Gas, hydrogen or helium, chromatographicgrade.7.2 Compressed Air, o
19、il-free.7.3 Hydrogen, chromatographic grade.7.4 Nitrogen, chromatographic grade.7.5 Pure Compounds for Calibrationn-Nonane, benzene,toluene, ethylbenzene, and o-xylene. The purity of the ethyl-benzene should be 99.8 % or better. The ethylbenzene must beanalyzed and corrections made in the compositio
20、n of thecalibration blend as required. The purity of all other com-pounds should be 99 % or greater. If the purity is less than99 %, the concentration and identification of the impuritiesmust be known so that the composition of the calibrationstandard can be adjusted for the presence of the impuriti
21、es.7.6 n-Undecane, for use as internal standard, 99 % orgreater purity.8. Hazards8.1 Consult current OSHA regulations, suppliers MaterialSafety Data Sheets, and local regulations for all materials usedin this test method.9. Sampling9.1 Guidelines for taking samples from bulk are given inPractice D 3
22、437.10. Calibration10.1 Prepare a calibration blend of each compound listed in7.5 and n-undecane at the 0.2 weight % level in ethylbenzeneas described in Practice D 4307. n-Nonane represents thenonaromatic hydrocarbons. A series of calibration blends thatspan the concentration range should be prepar
23、ed, one at theexpected level of impurities, another at one half the expectedlevel, and a third series at twice the expected level.10.2 Analyze the ethylbenzene used in preparing the cali-bration blend as described in 11.3.10.3 Analyze the calibration blend as described in 11.3.10.4 Calculate respons
24、e factors as follows:Ri5CiCs!SAiAs,i2AbAs,bD(1)where:Ri= response factor for impurity relative to internalstandard,Ai= area of impurity peak in calibration blend,Ab= area of impurity in ethylbenzene in calibrationblend,Cs= concentration of internal standard, weight %,As,i= area of internal standard
25、peak in calibration blend,As,b= area of internal standard peak in stock ethylben-zene, andCi= concentration of impurity, weight %.10.5 Calculate response factor to the nearest 0.001.11. Procedure11.1 Install the chromatographic column and establishstable instrument operation at the operating conditi
26、ons shownin Table 1. Refer to instructions provided by the manufacturerof the gas chromatograph and Practices E 355 and E 1510.11.2 Fill a 50-mL volumetric flask to the mark with testspecimen. With a microsyringe, add 30 L of the standard. Mixwell. Using a density of 0.740 for n-undecane and 0.867 f
27、orethylbenzene, this solution will contain 0.0512 weight %internal standard.11.3 Inject 0.6 L of solution into the gas chromatographand obtain the chromatogram. A typical chromatogram isshown in Fig. 1.12. Calculation12.1 Measure the areas of all peaks, including the internalstandard, except for the
28、 ethylbenzene peak.12.2 Sum all the peaks eluting before ethylbenzene exceptfor benzene, toluene, and the internal standard. Identify thissum as nonaromatic hydrocarbons.12.3 Calculate the weight percent of the individual impuri-ties, Ci, to the nearest 0.001 %, as follows:Ci50.0512 AiRiAs(2)where:A
29、i= area of impurity,Ri= response factor for impurity, andAs= area of internal standard.12.4 Use the response factor determined for o-xylene for allthe peaks eluting after ethylbenzene, and the response factordetermined for n-nonane for all the nonaromatic hydrocarbonpeaks.TABLE 1 Typical Instrument
30、ParametersCarrier gas heliumCarrier gas flow rate at 110C, mL/min 1.2Detector flame ionizationDetector temperature, C 240Injection port temperature, C 230Hydrogen flow rate, mL/min 30Airflow rate, mL/min 275Make-up gas nitrogenMake-up gas flow rate, mL/min 23Split flow, mL/min 150Column temperature,
31、 C 110Chart speed, cm/min 1Sample size, L 0.6D506007212.5 Calculate the purity of the ethylbenzene by subtractingthe sum of the impurities from 100.00.13. Report13.1 Report the following information:13.1.1 The concentration of each impurity to the nearest0.001 weight %, and13.1.2 The purity of ethyl
32、benzene to the nearest 0.01 weight%.14. Precision and Bias414.1 The following criteria should be used to judge theacceptability of the 95 % probability level of the resultsobtained by this test method. The criteria were derived from around robin between seven laboratories. The data were ob-tained ov
33、er two days using different operators.14.1.1 Intermediate PrecisionResults in the same labora-tory should not be considered suspect unless they differ bymore than the amount shown in Table 2.14.1.2 ReproducibilityThe results submitted by two labo-ratories should not be considered suspect unless they
34、 differ bymore than the amount shown in Table 2.14.2 BiasNo statement is made about bias since noacceptable reference material and value are available.15. Quality Guidelines15.1 Refer to Guide D 6809 for suggested QA/QC activitiesthat can be used as a part of this test method. It is recom-mended tha
35、t the operator of this test method select and performrelevant QA/QC activities like the ones in Guide D 6809 tohelp ensure the quality of data generated by this test method.16. Keywords16.1 ethylbenzene; ethylbenzene purity; impurities inethylbenzene4Supporting data have been filed at ASTM Internati
36、onal Headquarters and maybe obtained by requesting Research Report RR: D161030.FIG. 1 Typical Chromatogram (see Table 1)TABLE 2 Intermediate Precision and ReproducibilityComponentConcentration,Weight %IntermediatePrecisionReproducibilitysec-Butylbenzene 0.002 0.001 0.003n-Propylbenzene 0.010 0.002 0
37、.003m,p-Ethyltoluenes 0.014 0.003 0.002o-Xylene 0.013 0.004 0.007Cumene 0.012 0.003 0.002Benzene 0.024 0.004 0.005Toluene 0.592 0.083 0.100m,p-Xylene 0.090 0.024 0.019Diethylbenzenes 0.008 0.001 0.003Ethylbenzene 99.05 0.200 0.186D5060073SUMMARY OF CHANGESCommittee D16 has identified the location of
38、 selected changes to this standard since the last issue(D 5060 - 06) that may impact the use of this standard. (Approved January 1, 2007.)(1) Updated 2.1 to add reference to Practice E 1510 and GuideD 6809.(2) Added Section 5 on Interferences.(3) Modified 6.1 to require a minimum peak height respons
39、efrom 0.0010 wt% to be twice the height of the signalbackground noise.(4) Added Section 15 on QA/QC.ASTM 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 dete
40、rmination of the validity of any such patent rights, and the 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
41、 withdrawn. Your comments are invited either for revision of 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 tha
42、t your comments have not received a fair hearing you shouldmake 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).D5060074
