1、Designation: D 3160 07Standard Test Method forPhenol Content of Cumene (Isopropylbenzene) or AMS(aMethylstyrene)1This standard is issued under the fixed designation D 3160; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year o
2、f 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 covers the determination of phenol inrefined cumene (isopropylbenzene) or AMS (amethylsty-rene).1
3、.2 This test method has been found applicable in the rangefrom 5 to 50 mg/kg of phenol in refined cumene (isopropyl-benzene) or AMS (amethylstyrene).1.3 In determining the conformance of the test results usingthis method to applicable specifications, results shall berounded off in accordance with th
4、e rounding-off method ofPractice E29.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement 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 us
5、er of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see Section 7.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 3437 Practice for Samplin
6、g and Handling Liquid CyclicProductsD 6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications2.2 Other Document:OSHARegulations, 29 CFR paragraphs
7、 1910.000 and 1910,120033. Summary of Test Method3.1 The phenol content of cumene or AMS is determined bythe color development of phenol with 4-aminoantipyrine. Thesample absorbance is compared to phenol standards at 472 nmon a spectrophotometer.4. Significance and Use4.1 This test method is useful
8、in determining phenol in therange from 5 to 50 mg/kg in commercially available cumene orAMS.4.2 Phenol will inhibit certain reactions involving cumeneor AMS.5. Apparatus5.1 BalanceAny balance capable of measuring weights tothe nearest 0.001 g.5.2 SpectrophotometerAny spectrophotometer that canmeasur
9、e 0 to 2 absorbance units at 472 nm with a wavelengthrepeatability of 5 nm.5.3 Spectrophotometer Cells, 2 cm.5.4 Filter Paper.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent wa
10、ter as definedby Type I or II of Specification D 1193.6.3 Cumene or AMSWash 1 L of cumene or AMS with5 % aqueous sodium hydroxide ina2Lseparatory funnel.Discard the aqueous sodium hydroxide phase and filter thehydrocarbon through dry filter paper. Store the hydrocarbon1This test method is under the
11、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 June 1, 2007. Published June 2007. Originallyapproved in 1991. Last previous e
12、dition approved in 2003 as D 3160 03.2For 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 U.S. Gov
13、ernment 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 Conshohocken, PA 19428-
14、2959, United States.under a nitrogen blanket. The previous steps are taken to ensurethat the hydrocarbon will not contain phenol or peroxides.6.4 Solution of 4-Amino-AntipyrineDissolve 3.00 g ofamino-antipyrine in distilled water and dilute to volume in adark amber 100-mL volumetric flask. This shou
15、ld be stable fortwo weeks.6.5 Ammonium Persulfate SolutionDissolve 2.00 g ofammonium persulfate in distilled water and dilute to volume ina 100-mL volumetric flask. A fresh solution should be made upweekly.6.6 Ammonium Hydroxide, 0.880 specific gravity.6.7 Isopropyl Alcohol, reagent grade.6.8 Sodium
16、 Hydroxide, 5 % weight in distilled water.7. Hazards7.1 Some materials used in this test method are toxic orflammable, or both.7.2 If cumene has been exposed to air, cumene hydroper-oxide may be in the sample. Exercise suitable precautions forhandling cumene that may contain cumene hydroperoxide.7.3
17、 All glassware and equipment must be clean and free ofacid contamination.7.4 Cumene peroxides will decompose violently when incontact with strong acids.7.5 Sodium hydroxide is corrosive to the skin and eyes.7.6 Phenol is corrosive and toxic. Wear rubber gloves andchemical-type safety goggles, as a m
18、inimum.7.7 Isopropyl alcohol is flammable. Keep away from igni-tion sources.7.8 Consult current OSHA regulations, suppliers MaterialSafety Data Sheets, and local regulations for all materials usedin this test method.8. Sampling8.1 Sample the material in accordance with PracticeD 3437.8.2 Cumene will
19、 form peroxides when contacted with air.Sample and store cumene in air-tight containers.9. Preparation and Calibration of Standards9.1 Accurately weigh and transfer 0.100 g of phenol to a250-mL tared volumetric flask and bring the total net weight to100.00 g with phenol-free hydrocarbon as prepared
20、in 6.3.WarningSee 7.6. Mix well to dissolve. This is stockStandard Solution A (1000 mg/kg by weight).9.2 Transfer 0, 1, 2, 3, and 5 mL of Stock Solution A to a100-mL volumetric flask and dilute to volume with phenol-freehydrocarbon as prepared in 6.3 to yield 0, 10, 20, 30, and50-mg/kg solutions to
21、be named Solutions B, C, D, E, and Frespectively.9.3 Use the following procedure for Solutions B, C, D, E,and F:9.3.1 Accurately weigh and record 3.00 g of standardsolution in a 25-mL volumetric flask and add 5 mL of distilledwater and two drops of ammonium hydroxide. Mix well.9.3.2 Add 0.5 mL of 4-
22、amino-antipyrine solution followedby 0.5 mL of ammonium persulfate solution. Mix well and letstand for 10 min.9.3.3 Dilute to volume with isopropyl alcohol and mix well.WarningSee 7.7.9.3.4 Measure the absorbance of this solution at 472 nmusing a 2-cm cell against a blank, using Solution B.9.3.5 Plo
23、t a curve of absorbance versus milligram perkilogram phenol (sample size of 3.00 g).10. Procedure10.1 Use the procedure described in 9.3.1-9.3.4 using3.00-g sample instead of a standard solution.10.2 Obtain the milligram per kilogram phenol in thesample from the curve prepared in 9.3.5.NOTE 1This cu
24、rve assumes a sample size of 3 g.11. Calculation11.1 Calculate the phenol concentration in the sample withthe following equation:milligram per kilogram phenol 5C 3 3W(1)where:C = the concentration of phenol fora3gsample (from thecurve in 10.2), andW = the sample weight, g.11.2 To accommodate phenol
25、concentrations greater than 50mg/kg, adjust the original sample size to obtain a properabsorbance reading on the curve prepared in 9.3.5.Donotfurther dilute the final solution as this may cause turbidity.12. Report12.1 Report the concentration of phenol to the nearestmg/kg.13. Precision and Bias413.
26、1 PrecisionThe following criteria should be used tojudge the acceptability of the 95 % probability level of theresults obtained by this test method. The criteria were derivedfrom an interlaboratory study between three laboratories. Thedata were obtained over four days using different operators.The s
27、tudy was conducted at 5, 10, and 20 mg/kg of phenol.Reproducibility and intermediate precision may change athigher concentrations.13.1.1 Intermediate Precision (formerly calledRepeatability)Results in the same laboratory should not beconsidered suspect unless they differ by more than the follow-ing:
28、Level, mg/kg Intermediate Precision, mg/kg50.810 1.120 2.613.1.2 ReproducibilityResults submitted by two laborato-ries should not be considered suspect unless they differ bymore than the following:4Supporting data are available from ASTM International Headquarters. RequestRR: D161014.D3160072Level,
29、mg/kg Reproducibility, mg/kg51.110 2.720 5.313.2 BiasSince there is no accepted reference materialsuitable for determining the bias for the procedure in this testmethod, bias has not been determined.14. Quality Guidelines14.1 Refer to Guide D 6809 for suggested QA/QC activitiesthat can be used as a
30、part of the test method. It is recommendedthat the operator of this test method select and perform relevantQA/QC activities like the ones on Guide D 6809 to help ensurethe quality of the data generated by this test method.15. Keywords15.1 amethylstyrene; AMS; cumene; isopropylbenzene;phenol contentS
31、UMMARY OF CHANGESCommittee D16 has identified the location of selected changes to this standard since the last issue(D 3160 - 03) that may impact the use of this standard. (Approved June 1, 2007.)(1) Section 1 Former 1.1 divided into 1.1 and 1.2 perEditorial Guidelines and the rest renumbered. The r
32、ange in 1.2was adjusted to reflect actual precision and bias data for thelow level.(2) Section 2 Reference to Guide D 6809 was added.(3) Section 4 The range in 4.1 was adjusted to reflect actualprecision and bias data for the low level.(4) Section 5 References to some “ordinary” laboratoryitems were
33、 removed.(5) Sections 12 and 14 were added and sections renumberedaccordingly.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 valid
34、ity 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 withdrawn. Your comme
35、nts 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 that your comments have n
36、ot 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).D3160073
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