ASTM D3160-20a

Standard Test Method for Phenol Content of Cumene (Isopropylbenzene) or AMS (α–Methylstyrene)

SIGNIFICANCE AND USE
4.1 This test method is useful in determining phenol in the range from 5 to 50 mg/kg in commercially available cumene or AMS.  
4.2 Phenol will inhibit certain reactions involving cumene or AMS.
SCOPE
1.1 This test method covers the determination of phenol in refined cumene (isopropylbenzene) or AMS (α–methylstyrene).  
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 (α–methylstyrene). The limit of detection (LOD) is 0.9 mg/kg and the limit of quantitation (LOQ) is 2.9 mg/kg.
Note 1: LOD and LOQ were calculated using intermediate precision for the lowest level in the ILS.  
1.3 The following applies for the purposes of determining the conformance of the test results using this test method to applicable specifications, results shall be rounded off in accordance with 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 responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 7.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 30-Sep-2020
• ICS: 71.080.15 - Aromatic hydrocarbons
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.07 - Styrene, Ethylbenzene and C9 and C10 Aromatic Hydrocarbons

Relations

• Refers: ASTM D6809-02(2016) - Standard Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
• Effective Date: 01-Nov-2016
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2011
• Refers: ASTM D3437-11 - Standard Practice for Sampling and Handling Liquid Cyclic Products
• Effective Date: 01-Jan-2011
• Refers: ASTM D3437-10 - Standard Practice for Sampling and Handling Liquid Cyclic Products
• Effective Date: 01-Jun-2010
• Refers: ASTM E691-08 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Oct-2008
• Refers: ASTM E29-08 - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 01-Oct-2008
• Refers: ASTM D3437-08 - Standard Practice for Sampling and Handling Liquid Cyclic Products
• Effective Date: 01-Jun-2008
• Refers: ASTM D6809-02(2007) - Standard Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
• Effective Date: 01-Jun-2007
• Refers: ASTM E29-06b - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 15-Nov-2006
• Refers: ASTM E29-06a - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 15-Sep-2006
• Refers: ASTM E29-06 - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 01-May-2006
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM E691-05 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2005
• Refers: ASTM E29-04 - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 01-Dec-2004

Overview

ASTM D3160-20a is the recognized international standard for the determination of phenol content in refined cumene (isopropylbenzene) and α–methylstyrene (AMS). Issued by ASTM International, this test method is widely used in the chemical industry to measure phenol concentrations in the range of 5 to 50 mg/kg, ensuring product quality and supporting regulatory compliance. Phenol presence in cumene or AMS can inhibit certain reactions, making accurate detection critical for industrial processing and product performance.

This standard specifies a colorimetric method based on the reaction of phenol with 4-aminoantipyrine, followed by spectrophotometric measurement. The procedure is applicable to commercial samples of cumene and AMS, providing reliable quantitative results for both manufacturing and quality control environments.

Key Topics

• Test Method Range: Detects phenol between 5 and 50 mg/kg. The method offers a limit of detection (LOD) of 0.9 mg/kg and a limit of quantitation (LOQ) of 2.9 mg/kg.
• Industrial Relevance: Phenol is a potential inhibitor in the processing of cumene and α–methylstyrene. Its quantification is essential for process optimization and product specification.
• Spectrophotometric Analysis: Uses a color reaction with 4-aminoantipyrine to develop a measurable absorbance at 472 nm. Control of reagents and calibration standards are integral to accurate results.
• Quality Guidelines: Recommends laboratories to establish robust quality management and interlaboratory testing practices for reliability and comparability of data.
• Reporting and Compliance: Results are reported in SI units (mg/kg) and should be rounded per ASTM E29. Laboratories must account for safety, health, and environmental protocols during analysis.

Applications

• Raw Material Verification: Ensures that commercial cumene and AMS meet industry specifications for phenol content, minimizing reaction inhibition during further chemical processing.
• Quality Control: Essential for producers and buyers of cumene and AMS to verify material compliance with contractual or regulatory phenol thresholds.
• Process Optimization: By quantifying phenol impurities, manufacturers can optimize purification steps and reduce the risk of side reactions.
• Regulatory Compliance: The standard is referenced for fulfilling obligations related to occupational safety, health regulations, and international trade requirements.
• Research and Development: Supports analytical studies where phenol impurity profiling in aromatic hydrocarbons like cumene and AMS is required.

Related Standards

• ASTM D1193 – Specification for Reagent Water: Ensures the purity of water used in preparing reagents.
• ASTM D3437 – Practice for Sampling and Handling Liquid Cyclic Products: Provides techniques for representative sampling of materials like cumene and AMS.
• ASTM D6809 – Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials: Offers guidance on QA/QC methods for laboratories.
• ASTM E29 – Practice for Using Significant Digits in Test Data: Defines rounding procedures to ensure conformance with numerical reporting requirements.
• ASTM E691 – Practice for Conducting an Interlaboratory Study: Supports the determination of test method precision across multiple laboratories.

Keywords: ASTM D3160-20a, phenol content, cumene, isopropylbenzene, α–methylstyrene, AMS, spectrophotometry, quality control, chemical standard, aromatic hydrocarbons.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3160 − 20a
Standard Test Method for
Phenol Content of Cumene (Isopropylbenzene) or AMS
(α–Methylstyrene)
This standard is issued under the fixed designation D3160; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method covers the determination of phenol in 2.1 ASTM Standards:
refined cumene (isopropylbenzene) or AMS D1193 Specification for Reagent Water
(α–methylstyrene). D3437 Practice for Sampling and Handling Liquid Cyclic
Products
1.2 This test method has been found applicable in the range
D6809 Guide for Quality Control and Quality Assurance
from 5 to 50 mg/kg of phenol in refined cumene (isopropyl-
Procedures for Aromatic Hydrocarbons and Related Ma-
benzene) or AMS (α–methylstyrene). The limit of detection
terials
(LOD) is 0.9 mg/kg and the limit of quantitation (LOQ) is
E29 Practice for Using Significant Digits in Test Data to
2.9 mg⁄kg.
Determine Conformance with Specifications
NOTE 1—LOD and LOQ were calculated using intermediate precision
E691 Practice for Conducting an Interlaboratory Study to
for the lowest level in the ILS.
Determine the Precision of a Test Method
1.3 The following applies for the purposes of determining
2.2 Other Document:
the conformance of the test results using this test method to
OSHARegulations, 29 CFR paragraphs 1910.000 and 1910,
applicable specifications, results shall be rounded off in accor-
dance with the rounding-off method of Practice E29.
3. Summary of Test Method
1.4 The values stated in SI units are to be regarded as
3.1 The phenol content of cumene orAMS is determined by
standard. No other units of measurement are included in this
the color development of phenol with 4-aminoantipyrine. The
standard.
sample absorbance is compared to phenol standards at 472 nm
1.5 This standard does not purport to address all of the
on a spectrophotometer.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety, health, and environmental practices and deter-
4.1 This test method is useful in determining phenol in the
mine the applicability of regulatory limitations prior to use.
rangefrom5to50mg/kgincommerciallyavailablecumeneor
For specific hazard statements, see Section 7.
AMS.
1.6 This international standard was developed in accor-
4.2 Phenol will inhibit certain reactions involving cumene
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the or AMS.
Development of International Standards, Guides and Recom-
5. Apparatus
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 5.1 Balance—Any balance capable of measuring weights to
the nearest 0.001 g.
1 2
This test method is under the jurisdiction of ASTM Committee D16 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi- contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
bility of Subcommittee D16.07 on Styrene, Ethylbenzene and C9 and C10Aromatic Standards volume information, refer to the standard’s Document Summary page on
Hydrocarbons. the ASTM website.
Current edition approved Oct. 1, 2020. Published October 2020. Originally Available from Superintendent of Documents, U.S. Government Printing
approved in 1991. Last previous edition approved in 2020 as D3160 – 20. DOI: Office, 732 N. Capitol St. NW, Mail Stop: SDE, Washington, DC 20401.,
10.1520/D3160-20A. http://www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3160 − 20a
5.2 Spectrophotometer—Any spectrophotometer that can 7.3 All glassware and equipment must be clean and free of
measure 0 to 2 absorbance units at 472 nm with a wavelength acid contamination.
repeatability of 5 nm.
7.4 Cumene peroxides will decompose violently when in
5.3 Spectrophotometer Cells, 2 cm. contact with strong acids.
5.4 Filter Paper.
7.5 Sodium hydroxide is corrosive to the skin and eyes.
7.6 Phenol is corrosive and toxic. Wear rubber gloves and
6. Reagents and Materials
chemical-type safety goggles, as a minimum.
6.1 Purity of Reagents—Reagent grade chemicals shall be
7.7 Isopropyl alcohol is flammable. Keep away from igni-
used in all tests. Unless otherwise indicated, it is intended that
tion sources.
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society, 7.8 Consult current OSHA regulations, suppliers’ Safety
where such specifications are available. Other grades may be
Data Sheets, and local regulations for all materials used in this
used, provided it is first ascertained that the reagent is of test method.
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
8. Sampling
6.2 Purity of Water—Unless otherwise indicated, references
8.1 Sample the material in accordance with Practice D3437.
to water shall be understood to mean reagent water as defined
8.2 Cumene will form peroxides when contacted with air.
by Type I or II of Specification D1193. Type I is the highest
Sample and store cumene in air-tight containers.
purity with a maximum conductivity of 0.056 µS/cm. Type II
water requires distillation. Type III water has a maximum
9. Preparation and Calibration of Standards
conductivity of 0.25 µS/cm and there are significant quantities
9.1 Transfer approximately 0.1 g of phenol to a 250-mL
of other impurities. Type IV water has a maximum conductiv-
taredvolumetricflaskandrecordtheweight.Bringthetotalnet
ity of 5 µS/cm and unlimited quantities of TOC and silica.
weight to approximately 100 g with phenol-free hydrocarbon
6.3 Cumene or AMS—Wash 1 L of cumene or AMS with
as prepared in 6.3. Warning—See 7.6. Mix well to dissolve.
5 % aqueous sodium hydroxide ina2L separatory funnel.
This is stock Standard Solution A whose phenol concentration
Discard the aqueous sodium hydroxide phase and filter the
should be expressed as mg/kg by weight based on the actual
hydrocarbon through dry filter paper. Store the hydrocarbon
amounts of phenol and phenol-free hydrocarbon used.
underanitrogenblanket.Thepreviousstepsaretakentoensure
9.2 Transfer 0, 1, 2, 3, and 5 mL of Stock Solution A to a
that the hydrocarbon will not contain phenol or peroxides.
100-mLvolumetricflaskanddilutetovolumewithphenol-free
6.4 Solution of 4-Amino-Antipyrine—Dissolve 3.00 g of
hydrocarbon as prepared in 6.3 to yield approximately 0, 10,
amino-antipyrine in distilled water and dilute to volume in a
20, 30, and 50-mg/kg solutions to be named Solutions B, C, D,
dark amber 100-mLvolumetric flask. This should be stable for
E, and F respectively. Calculate the actual mg/kg phenol
two weeks.Alternate volumes of solutions may be prepared so
...

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 previous version. Because
it 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 version
of the standard as published by ASTM is to be considered the official document.
Designation: D3160 − 20 D3160 − 20a
Standard Test Method for
Phenol Content of Cumene (Isopropylbenzene) or AMS
(α–Methylstyrene)
This standard is issued under the fixed designation D3160; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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 (α–methylstyrene).
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 (α–methylstyrene). The limit of detection (LOD) is 0.9 mg/kg and the limit of quantitation (LOQ) is 2.9 2.9 mg mg/kg.⁄kg.
NOTE 1—LOD and LOQ were calculated using intermediate precision for the lowest level in the ILS.
1.3 The following applies for the purposes of determining the conformance of the test results using this test method to applicable
specifications, results shall be rounded off in accordance with 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 responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. For specific hazard statements, see Section 7.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D3437 Practice for Sampling and Handling Liquid Cyclic Products
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsibility of
Subcommittee D16.07 on Styrene, Ethylbenzene and C9 and C10 Aromatic Hydrocarbons.
Current edition approved July 1, 2020Oct. 1, 2020. Published July 2020October 2020. Originally approved in 1991. Last previous edition approved in 20162020 as
D3160 – 16.D3160 – 20. DOI: 10.1520/D3160-20.10.1520/D3160-20A.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3160 − 20a
2.2 Other Document:
OSHA Regulations, 29 CFR paragraphs 1910.000 and 1910, 1200
3. Summary of Test Method
3.1 The phenol content of cumene or AMS is determined by the color development of phenol with 4-aminoantipyrine. The sample
absorbance is compared to phenol standards at 472 nm on a spectrophotometer.
4. Significance and Use
4.1 This test method is useful in determining phenol in the range from 5 to 50 mg/kg in commercially available cumene or AMS.
4.2 Phenol will inhibit certain reactions involving cumene or AMS.
5. Apparatus
5.1 Balance—Any balance capable of measuring weights to the nearest 0.001 g.
5.2 Spectrophotometer—Any spectrophotometer that can measure 0 to 2 absorbance units at 472 nm with a wavelength
repeatability of 5 nm.
5.3 Spectrophotometer Cells, 2 cm.
5.4 Filter Paper.
6. Reagents and Materials
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by Type
I or II of Specification D1193. Type I is the highest purity with a maximum conductivity of 0.056 μS/cm. Type II water requires
distillation. Type III water has a maximum conductivity of 0.25 μS/cm and there are significant quantities of other impurities. Type
IV water has a maximum conductivity of 5 μS/cm and unlimited quantities of TOC and silica.
6.3 Cumene or AMS—Wash 1 L of cumene or AMS with 5 % aqueous sodium hydroxide in a 2 L separatory funnel. Discard the
aqueous sodium hydroxide phase and filter the hydrocarbon through dry filter paper. Store the hydrocarbon under a nitrogen
blanket. The previous steps are taken to ensure that the hydrocarbon will not contain phenol or peroxides.
6.4 Solution of 4-Amino-Antipyrine—Dissolve 3.00 g of amino-antipyrine in distilled water and dilute to volume in a dark amber
100-mL volumetric flask. This should be stable for two weeks. Alternate volumes of solutions may be prepared so long as the
preparation meets the concentration specified.
6.5 Ammonium Persulfate Solution—Dissolve 2.00 g of ammonium persulfate in distilled water and dilute to volume in a 100-mL
volumetric flask. A fresh solution should be made up weekly. Alternate volumes of solutions may be prepared so long as the
preparation meets the concentration specified.
6.6 Ammonium Hydroxide, 0.880 specific gravity.
Available from Superintendent of Documents, U.S. Government Printing Office, 732 N. Capitol St. NW, Mail Stop: SDE, Washington, DC 20401., http://
www.access.gpo.gov.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference Materials, American Chemical Society, Washington, DC. For
suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D3160 − 20a
6.7 Isopropyl Alcohol, reagent grade.
6.8 Sodium Hydroxide, 5 % weight in distilled water.
7. Hazards
7.1 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 precautions for handling
cumene 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 corr
...