1、Designation: D5060 12Standard Test Method forDetermining Impurities in High-Purity Ethylbenzene by GasChromatography1This standard is issued under the fixed designation D5060; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r 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. Scope*1.1 This test method describes the analysis of normallyoccurring impurities in, and the purity of, ethylbenzene by g
3、aschromatography. 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-xylene m
4、ay 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 The values stated in SI units are to be regarded asstandard. No other units of measuremen
5、t are included in thisstandard.1.5 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 limitatio
6、ns prior to use. For a specifichazard statement, see Section 8.2. Referenced Documents2.1 ASTM Standards:2D3437 Practice for Sampling and Handling Liquid CyclicProductsD4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD6809 Guide for Quality Control and Quality AssuranceP
7、rocedures for Aromatic Hydrocarbons and Related Ma-terialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE355 Practice for Gas Chromatography Terms and Relation-shipsE1510 Practice for Installing Fused Silica Open TubularCapillary Columns in Gas Chr
8、omatographs2.2 Other Documents:OSHA Regulations, 29 CFR paragraphs 1910.1000 and1910.120033. Summary of Test Method3.1 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 anal
9、ysis. The impurities are measured relative to theinternal standard. Ethylbenzene purity is calculated by sub-tracting 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 whereet
10、hylbenzene is used in manufacturing processes. It may beused in development or research work involving ethylbenzene.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
11、 A key operational parameter for this method is theseparation of p-xylene from ethylbenzene. Care should betaken during 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 slig
12、htly until separation is achieved.1This test method is 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 AromaticHydrocarbons.Current edition approved June 1, 2012.
13、 Published August 2012. Originallyapproved in 1990. Last previous edition approved in 2007 as D5060 07. DOI:10.1520/D5060-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information,
14、refer to the standards Document Summary page onthe ASTM website.3Available 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.*A Summary of Changes section appears at the end of this standardCopyrigh
15、t ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Apparatus6.1 Gas Chromatograph (GC)any GC built for capillarycolumn chromatography and equipped with a flame ionizationdetector (FID). The system shall have sufficient sensitivity,linearity,
16、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 eitherthe detector or the electronic integration for the major compo-nents. It shall have a split injection system that will notdiscrimin
17、ate over the boiling range of the samples analyzed.6.2 Chromatographic Column, fused silica capillary, 60 mlong, 0.32-mm inside diameter, 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 c
18、apable of separating all major impurities andthe internal standard from the ethylbenzene under operatingconditions appropriate for the column.6.3 Chromatographic Data System is required.6.4 Microsyringe, 10-L.6.5 Microsyringe, 50-L.6.6 Volumetric Flask, 50-mL.7. Reagents and Materials7.1 Carrier Gas
19、, hydrogen or helium, chromatographicgrade.7.2 Compressed Air, oil-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 eth
20、ylbenzene must beanalyzed and corrections made in the composition 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 cali
21、brationstandard can be adjusted for the presence of the impurities.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
22、Guidelines for taking samples from bulk are given inPractice D3437.10. Calibration10.1 Prepare a calibration standard of ethylbenzene withimpurities (listed in 7.5) at concentrations representative ofthose expected in the samples to be analyzed as described inPractice D4307.10.2 Fill a 50-mL volumet
23、ric flask partially with the cali-bration standard. With a microsyringe, add 30 L of theinternal standard n-undecane, and make up to the mark with thecalibration standard. Mix well. Using a density of 0.740 forn-undecane and 0.867 for the calibration standard, this calibra-tion blend will contain 0.
24、0512 weight % internal standard.10.3 Fill a 50-mL volumetric flask to the mark with ethyl-benzene. With a microsyringe add 30 L (or proper size) of theinternal standard n-undecane. Mix well. The resulting stockethylbenzene solution will contain 0.0512 weight % internalstandard.10.4 Analyze the calib
25、ration blend (10.2) as described in11.3.10.5 Analyze the stock ethylbenzene solution (10.3)asdescribed in 11.3.10.6 Calculate response factors as follows:Ri5CiCs!SAiAs,i2AbAs,bD(1)where:Ri= response factor for impurity i relative to internalstandard,Ai= peak area of impurity i in calibration blend,A
26、b= peak area of impurity i in stock ethylbenzene solution,Cs= concentration of internal standard,As,i= peak area of internal standard in calibration blend,As,b= peak area of internal standard in stock ethylbenzenesolution, andCi= concentration of impurity i, weight %.10.7 Calculate response factor t
27、o the nearest 0.001.11. Procedure11.1 Install the chromatographic column and establishstable instrument operation at the operating conditions shownin Table 1. Refer to instructions provided by the manufacturerof the gas chromatograph and Practices E355 and E1510.11.2 Fill a 50-mL volumetric flask to
28、 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 forethylbenzene, this solution will contain 0.0512 weight %internal standard.TABLE 1 Typical Instrument ParametersCarrier gas heliumCarrier gas flow rate at 110C, mL
29、/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, C 110Chart speed, cm/min 1Sample size, L 0.6D5060 12211.3 In
30、ject 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 ethylbenzene peak.12.2 Sum all the peaks eluting before ethylbenzene exceptfor ben
31、zene, 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:Ci5 Cs3 Ai3 Ri As(2)where:Cs= concentration of internal standard, weight %,Ai= peak area of impurity i,Ri= re
32、sponse factor for impurity i, andAs= peak 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.12.5 Calculate the purity of the ethylbenzene
33、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 ethylbenzene to the nearest 0.01 weight%.14. Precision and Bias414.1 The following criteria should be us
34、ed 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 over two days using different operators.14.1.1 Intermediate PrecisionResults in the same labora-tory
35、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 differ bymore than the amount shown in Table 2.14.2 BiasNo statement is made about bias since noac
36、ceptable reference material and value are available.15. Quality Guidelines15.1 Laboratories shall have a quality control system inplace.15.1.1 Confirm the performance of the test instrument ortest method by analyzing a quality control sample followingthe guidelines of standard statistical quality co
37、ntrol practices.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D16-1030.FIG. 1 Typical Chromatogram (see Table 1)D5060 12315.1.2 A quality control sample is a stable material isolatedfrom the production process and representati
38、ve of the samplebeing analyzed.15.1.3 When QA/QC protocols are already established inthe testing facility, these protocols are acceptable when theyconfirm the validity of test results.15.1.4 When there are no QA/QC protocols established inthe testing facility, use the guidelines described in GuideD6
39、809 or similar statistical quality control practices.16. Keywords16.1 ethylbenzene; ethylbenzene purity; impurities inethylbenzeneSUMMARY OF CHANGESCommittee D16 has identified the location of selected changes to this standard since the last issue (D5060 - 07)that may impact the use of this standard
40、. (Approved June 1, 2012.)(1) Added Section 1.4 on SI units.(2) Replaced Section 6.3 recorder with chromatographic datasystem.(3) Modified Section 10 on Calibration.(4) Modified the definition of symbols in Equations 1 and 2.(5) Modified Equation 2 in Section 12.(6) Replaced Section 15 on Quality wi
41、th the latest editorialguidelines.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 determination of the validity of any such patent rights, and the risko
42、f 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 of this
43、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 shouldmake yo
44、ur 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 co
45、ntacting 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 2 Intermediate Precision and
46、 ReproducibilityComponentConcentration,Weight %IntermediatePrecisionReproducibilitysec-Butylbenzene 0.002 0.001 0.003n-Propylbenzene 0.010 0.002 0.003m,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 0.186D5060 124
