1、Designation: D3160 12D3160 16Standard Test Method forPhenol Content of Cumene (Isopropylbenzene) or AMS(Methylstyrene)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 y
2、ear 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 covers the determination of phenol in refined cumene (isopropylbenzene) or AMS (methylstyrene
3、).1.2 This test method has been found applicable in the range from 5 to 50 mg/kg of phenol in refined cumene (isopropylbenzene)or AMS (methylstyrene).1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be roundedoff in accordance with
4、the rounding-off method of Practice E29.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof
5、the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific hazard statements, see Section 7.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD3437 Practice for Sampl
6、ing and Handling Liquid Cyclic ProductsD6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related MaterialsE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE691 Practice for Conducting an Interlaboratory St
7、udy to Determine the Precision of a Test Method2.2 Other Document:OSHA Regulations, 29 CFR paragraphs 1910.000 and 1910, 1200 33. Summary of Test Method3.1 The phenol content of cumene or AMS is determined by the color development of phenol with 4-aminoantipyrine. Thesample absorbance is compared to
8、 phenol standards at 472 nm on a spectrophotometer.4. Significance and Use4.1 This test method is useful in determining phenol in the range from 5 to 50 mg/kg in commercially available cumene orAMS.4.2 Phenol will inhibit certain reactions involving cumene or AMS.5. Apparatus5.1 BalanceAny balance c
9、apable of measuring weights to the nearest 0.001 g.5.2 SpectrophotometerAny spectrophotometer that can measure 0 to 2 absorbance units at 472 nm with a wavelengthrepeatability of 5 nm.1 This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons and Related Chemicals an
10、d is the direct responsibility of SubcommitteeD16.07 on Styrene, Ethylbenzene and C9 and C10 Aromatic Hydrocarbons.Current edition approved March 1, 2012June 1, 2016. Published March 2012June 2016. Originally approved in 1991. Last previous edition approved in 20072012 asD3160 07.D3160 12. DOI: 10.1
11、520/D3160-12.10.1520/D3160-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standardsstandards Document Summary page on the ASTM website.3 Available from U.S.
12、Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previo
13、us version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Chang
14、es section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.3 Spectrophotometer Cells, 2 cm.5.4 Filter Paper.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall be used. Unless otherwise
15、indicated, it is intended that all reagents shallconform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where suchspecifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
16、to permit its use without lessening the accuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined byType I or II of Specification D1193. Type I is the highest purity with a maximum conductivity of 0.056 S/cm.
17、 Type II waterrequires distillation. Type III water has a maximum conductivity of 0.25 S/cm and there are significant quantities of otherimpurities. Type IV water has a maximum conductivity of 5 S/cm and unlimited quantities of TOC and silica.6.3 Cumene or AMSWash 1 L of cumene or AMS with 5 % aqueo
18、us sodium hydroxide in a 2 L separatory funnel. Discardthe aqueous sodium hydroxide phase and filter the hydrocarbon through dry filter paper. Store the hydrocarbon under a nitrogenblanket. The previous steps are taken to ensure that the hydrocarbon will not contain phenol or peroxides.6.4 Solution
19、of 4-Amino-AntipyrineDissolve 3.00 g of amino-antipyrine in distilled water and dilute to volume in a dark amber100-mL volumetric flask. This should be stable for two weeks. Alternate volumes of solutions may be prepared so long as thepreparation meets the concentration specified.6.5 Ammonium Persul
20、fate SolutionDissolve 2.00 g of ammonium persulfate in distilled water and dilute to volume in a100-mL volumetric flask. A fresh solution should be made up weekly. Alternate volumes of solutions may be prepared so long asthe preparation meets the concentration specified.6.6 Ammonium Hydroxide, 0.880
21、 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 or flammable, or both.7.2 If cumene has been exposed to air, cumene hydroperoxide may be in the sample. Exercise suitable precaut
22、ions for handlingcumene that may contain cumene hydroperoxide.7.3 All glassware and equipment must be clean and free of acid contamination.7.4 Cumene peroxides will decompose violently when in contact with strong acids.7.5 Sodium hydroxide is corrosive to the skin and eyes.7.6 Phenol is corrosive an
23、d toxic. Wear rubber gloves and chemical-type safety goggles, as a minimum.7.7 Isopropyl alcohol is flammable. Keep away from ignition sources.7.8 Consult current OSHA regulations, suppliers Material suppliersSafety Data Sheets, and local regulations for all materialsused in this test method.8. Samp
24、ling8.1 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-mL tared volumetric flask and record th
25、e weight. Bring the total net weightto approximately 100 g with phenol-free hydrocarbon as prepared in 6.3. WarningSee 7.6. Mix well to dissolve. This is stockStandard Solution A whose phenol concentration should be expressed as mg/kg by weight based on the actual amounts of phenoland phenol-free hy
26、drocarbon used.9.2 Transfer 0, 1, 2, 3, and 5 mL of Stock Solution A to a 100-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 respectively. Calculate the actual
27、 mg/kg phenol concentrations based on the weights in 9.1.4 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH
28、 Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial convention, Inc. (USPC), Rockville, MD.D3160 1629.3 Use the following procedure for Solutions B, C, D, E, and F:9.3.1 Accurately weigh and record 3.00 g of standard solution in a 25-mL volumetric
29、 flask and add 5 mL of distilled water andtwo drops of ammonium hydroxide. Mix well.9.3.2 Add 0.5 mL of 4-amino-antipyrine solution followed by 0.5 mL of ammonium persulfate solution. Mix well and let standfor 10 min.9.3.3 Dilute to volume with isopropyl alcohol and mix well. WarningSee 7.7.9.3.4 Me
30、asure the absorbance of this solution at 472 nm using a 2-cm cell against a blank, using Solution B.9.3.5 Plot a curve of absorbance versus milligram per kilogram phenol (sample size of 3.00 g).10. Procedure10.1 Use the procedure described in 9.3.1 9.3.4 using approximately 3 g of sample instead of
31、a standard solution.10.2 Obtain the milligram per kilogram phenol in the sample from the curve prepared in 9.3.5.NOTE 1This curve assumes a sample size of 3.00 g as described in 9.3.5. The adjusted, actual, mg/kg is calculated as described in Section 11.11. Calculation11.1 Calculate the phenol conce
32、ntration in the sample adjusted for the actual sample weight versus the 3.00 standard curve withthe following equation:milligram per kilogram phenol5C 33.00 gW (1)where:C = the concentration of phenol for a 3.00 g sample (from the curve in 10.2) andW = the sample weight, g.where:C = the concentratio
33、n of phenol for a 3.00 g sample (from the curve in 10.2) andW = the sample weight, g.11.2 To accommodate phenol concentrations greater than 50 mg/kg, adjust the original sample size to obtain a properabsorbance reading on the curve prepared in 9.3.5 and generate the actual phenol concentration using
34、 Eq 1 where W will be lessthan 3 g. Do not further dilute the final solution as this may cause turbidity.12. Report12.1 Report the concentration of phenol to the nearest mg/kg.13. Precision and Bias513.1 PrecisionThe following criteria should be used to judge the acceptability of the 95 % probabilit
35、y level of the resultsobtained by this test method. The criteria were derived from an interlaboratory study between three laboratories. The data wereobtained over four days using different operators. The study was conducted at 5, 10, and 20 mg/kg of phenol. The details are givenin Research Report RR
36、:D16-1014. It should be noted that the ILS did not meet the minimum requirements of Practice E691.Reproducibility and intermediate precision may change at higher concentrations.13.1.1 Intermediate Precision (formerly called Repeatability)Results in the same laboratory should not be considered suspec
37、tunless they differ by more than the following:following.Results differing by less than “r” have a 95 % probability of being correct:Level, mg/kg Intermediate Precision, mg/kgLevel, mg/kg Intermediate Precision (r), mg/kg5 0.810 1.120 2.613.1.2 ReproducibilityResults submitted by two laboratories sh
38、ould not be considered suspect unless they differ by more thanthe following: following. Results differing by less than “R” have a 95 % probability of being correct:Level, mg/kg Reproducibility, mg/kgLevel, mg/kg Reproducibility (R), mg/kg5 1.110 2.720 5.35 Supporting data have been filed at ASTM Int
39、ernational Headquarters and may be obtained by requesting Research Report RR:D16-1014. Contact ASTM CustomerService at serviceastm.org.D3160 16313.2 BiasSince there is no accepted reference material suitable for determining the bias for the procedure in this test method,bias has not been determined.
40、14. Quality Guidelines14.1 Laboratories shall have a quality control system in place.14.1.1 Confirm the performance of the test instrument or test method by analyzing a quality control sample following theguidelines of standard statistical quality control practices.14.1.2 Aquality control sample is
41、a stable material isolated from the production process and representative of the sample beinganalyzed.14.1.3 When QA/QC protocols are already established in the testing facility, these protocols are acceptable when they confirmthe validity of test results.14.1.4 When there are no QA/QC protocols est
42、ablished in the testing facility, use the guidelines described in Guide D6809 orsimilar statistical quality control practices.15. Keywords15.1 methylstyrene; AMS; cumene; isopropylbenzene; phenol contentSUMMARY OF CHANGESCommittee D16 has identified the location of selected changes to this standard
43、since the last issue(D3160 - 07D3160)12) that may impact the use of this standard. (Approved MarchJune 1, 2012.)2016.)(1) Sections 9 11 were reworded to be clearer in the approach and intent of the procedure and calculations.Section 2.1: Addedreference to E691.(2) Section 7: Changed MSDS to SDS.(3)
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