1、Designation: D3160 12Standard Test Method forPhenol Content of Cumene (Isopropylbenzene) or AMS(aMethylstyrene)1This standard is issued under the fixed designation D3160; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、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 covers the determination of phenol inrefined cumene (isopropylbenzene) or AMS(amethylstyrene).1.2 Th
3、is 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 the rou
4、nding-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 user of
5、 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:2D1193 Specification for Reagent WaterD3437 Practice for Sampling and H
6、andling Liquid CyclicProductsD6809 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 1910.00
7、0 and 1910,120033. Summary of Test Method3.1 The phenol content of cumene orAMS 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 in determ
8、ining 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 canmeasure 0 to 2
9、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. Unless otherwise indicated, it is intended that all reagentsshall conform to the specifications of the Committee
10、 onAnalytical Reagents of the American Chemical Society, wheresuch specifications are available.4Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.1This test method is under th
11、e 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 March 1, 2012. Published March 2012. Originallyapproved in 1991. Last previo
12、us edition approved in 2007 as D3160 07. DOI:10.1520/D3160-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website
13、.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.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing o
14、f reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial convention, Inc. (USPC), Rockville,MD.1*A Summary of Changes section appears at the end of
15、this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type I or II of Specification D1193. Type I is the
16、highestpurity with a maximum conductivity of 0.056 S/cm. Type IIwater requires distillation. Type III water has a maximumconductivity of 0.25 S/cm and there are significant quantitiesof other impurities. Type IV water has a maximum conductiv-ity of 5 S/cm and unlimited quantities of TOC and silica.6
17、.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 hydrocarbonunder a nitrogen blanket. The previous steps are taken to ensurethat the hydrocarbon w
18、ill 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 should be stable fortwo weeks. Alternate volumes of solutions may be prepared solong as the preparation meets
19、the concentration specified.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. Alternate volumes of solutions may be prepared solong as the preparation meets the concentr
20、ation specified.6.6 Ammonium Hydroxide, 0.880 specific gravity.6.7 Isopropyl Alcohol, reagent grade.6.8 Sodium 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 ma
21、y be in the sample. Exercise suitable precautions forhandling cumene that may contain cumene hydroperoxide.7.3 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 t
22、he skin and eyes.7.6 Phenol is corrosive and toxic. Wear rubber gloves andchemical-type safety goggles, as a minimum.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 material
23、s usedin this test method.8. Sampling8.1 Sample the material in accordance with Practice D3437.8.2 Cumene will form peroxides when contacted with air.Sample and store cumene in air-tight containers.9. Preparation and Calibration of Standards9.1 Transfer approximately 0.1 g of phenol to a 250-mLtared
24、 volumetric flask and record the weight. Bring the total netweight to approximately 100 g with phenol-free hydrocarbonas prepared in 6.3. WarningSee 7.6. Mix well to dissolve.This is stock Standard Solution A whose phenol concentrationshould be expressed as mg/kg by weight based on the actualamounts
25、 of phenol and phenol-free hydrocarbon used.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 approximately 0, 10,20, 30, and 50-mg/kg solutions to be named Solutions B, C, D,E, and F respect
26、ively. Calculate the actual mg/kg phenolconcentrations based on the weights in 9.1.9.3 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 hydroxid
27、e. Mix well.9.3.2 Add 0.5 mL of 4-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
28、 blank, using Solution B.9.3.5 Plot 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 using ap-proximately3gofsample instead of a standard solution.10.2 Obtain the milligram per kilogram phenol in thesample
29、from the curve prepared in 9.3.5.NOTE 1This curve assumes a sample size of 3.00 g as described in9.3.5. The adjusted, actual, mg/kg is calculated as described in Section 11.11. Calculation11.1 Calculate the phenol concentration in the sample ad-justed for the actual sample weight versus the 3.00 sta
30、ndardcurve with the following equation:milligram per kilogram phenol 5C 3 3.00 gW(1)where:C = the concentration of phenol for a 3.00 g sample (fromthe curve in 10.2) andW = the sample weight, g.11.2 To accommodate phenol concentrations greater than 50mg/kg, adjust the original sample size to obtain
31、a properabsorbance reading on the curve prepared in 9.3.5 and generatethe actual phenol concentration using Eq 1 where W will beless than 3 g. Do not further dilute the final solution as this maycause turbidity.12. Report12.1 Report the concentration of phenol to the nearestmg/kg.13. Precision and B
32、ias513.1 PrecisionThe following criteria should be used tojudge the acceptability of the 95 % probability level of the5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D16-1014.D3160 122results obtained by this test method. The cr
33、iteria were derivedfrom an interlaboratory study between three laboratories. Thedata were obtained over four days using different operators.The study was conducted at 5, 10, and 20 mg/kg of phenol.Reproducibility and intermediate precision may change athigher concentrations.13.1.1 Intermediate Preci
34、sion (formerly calledRepeatability)Results in the same laboratory should not beconsidered suspect unless they differ by more than the follow-ing: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 unl
35、ess they differ bymore than the following:Level, 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 Laboratories shall have a
36、 quality control system inplace.14.1.1 Confirm the performance of the test instrument ortest method by analyzing a quality control sample followingthe guidelines of standard statistical quality control practices.14.1.2 A quality control sample is a stable material isolatedfrom the production process
37、 and representative of the samplebeing analyzed.14.1.3 When QA/QC protocols are already established inthe testing facility, these protocols are acceptable when theyconfirm the validity of test results.14.1.4 When there are no QA/QC protocols established inthe testing facility, use the guidelines des
38、cribed in GuideD6809 or similar statistical quality control practices.15. Keywords15.1 amethylstyrene; AMS; cumene; isopropylbenzene;phenol contentSUMMARY OF CHANGESCommittee D16 has identified the location of selected changes to this standard since the last issue (D3160 - 07)that may impact the use
39、 of this standard. (Approved March 1, 2012.)(1) Sections 9 11 were reworded to be clearer in the approachand intent of the procedure and calculations.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. User
40、s of this standard are expressly advised that determination 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
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42、l committee, which you may attend. If you feel that 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,
43、 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D3160 123
