ASTM D7065-17

Standard Test Method for Determination of Nonylphenol, Bisphenol A, <emph type="bdit" >p-tert</emph>-Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters by Gas Chromatography Mass Spectrometry

SIGNIFICANCE AND USE
5.1 Nonylphenol,4 octylphenol, and bisphenol A have been shown to have toxic effects in aquatic organisms. The source of nonylphenol and octylphenol is prominently from the use of common commercial surfactants. The most widely used surfactant is NPEO which has an average ethoxylate chain of 9 mol of ethoxylate. The ethoxylate chain is readily biodegraded to form NP1EO and NP2EO, nonylphenol carboxylate (NPEC) and, under anaerobic conditions, nonylphenol. Nonylphenol will also biodegrade, but may be released into environmental waters directly at trace levels. This test method has been investigated for use with surface water and waste treatment effluent samples and is applicable to these matrices. It has not been investigated for use with salt water or solid sample matrices.  
5.2 The first reported synthesis of BPA was by the reaction of phenol with acetone by Zincke.5 BPA has become an important high volume industrial chemical used in the manufacture of polycarbonate plastics and epoxy resins. Polycarbonate plastic and resins are used in numerous products including electrical and electronic equipment, automobiles, sports and safety equipment, reusable food and drink containers, electrical laminates for printed circuit boards, composites, paints, adhesives, dental sealants, protective coatings, and many other products.6 The environmental source of BPA is predominantly from the decomposition of polycarbonate plastics and resins. BPA is not classified as bio-accumulative by the U.S. Environmental Protection Agency (EPA) and will biodegrade. BPA may be released into the environment waters directly at trace levels through landfill leachate and sewage treatment plant effluents.
SCOPE
1.1 This test method covers determination of nonylphenol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), octylphenol (OP), and bisphenol A (BPA) that are partitioned into organic solvent, separated using gas chromatography and detected with mass selective detection. These compounds or isomer mixtures are qualitatively and quantitatively determined by this test method. This test method adheres to selected ion monitoring mass spectrometry but full scan mass spectrometry has also been shown to work well under these conditions. Either analysis may be used.  
1.2 The method detection limit (MDL) and reporting limit (RL) for NP, NP1EO, NP2EO, OP, and BPA are listed in Table 1. (A) MDL determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B.(B) Lowest point of the reporting range is calculated from the LV1 concentration calibration standard in Table 4.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.  
1.5 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: 14-Dec-2017
• ICS: 71.080.15 - Aromatic hydrocarbons
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Relations

• Referred By: ASTM F2931-19a - Standard Guide for Analytical Testing of Substances of Very High Concern in Materials and Products
• Effective Date: 15-Dec-2017

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: D7065 − 17
Standard Test Method for
Determination of Nonylphenol, Bisphenol A, p-tert-
Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol
Diethoxylate in Environmental Waters by Gas
1
Chromatography Mass Spectrometry
This standard is issued under the fixed designation D7065; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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
2
1.1 This test method covers determination of nonylphenol 2.1 ASTM Standards:
(NP), nonylphenol ethoxylate (NP1EO), nonylphenol di- D1129Terminology Relating to Water
ethoxylate(NP2EO),octylphenol(OP),andbisphenolA(BPA) D1193Specification for Reagent Water
that are partitioned into organic solvent, separated using gas D3694Practices for Preparation of Sample Containers and
chromatography and detected with mass selective detection. for Preservation of Organic Constituents
These compounds or isomer mixtures are qualitatively and D3856Guide for Management Systems in Laboratories
quantitativelydeterminedbythistestmethod.Thistestmethod Engaged in Analysis of Water
adheres to selected ion monitoring mass spectrometry but full D5847Practice for Writing Quality Control Specifications
scan mass spectrometry has also been shown to work well for Standard Test Methods for Water Analysis
under these conditions. Either analysis may be used. D5905Practice for the Preparation of SubstituteWastewater
E691Practice for Conducting an Interlaboratory Study to
1.2 The method detection limit (MDL) and reporting limit
Determine the Precision of a Test Method
(RL) for NP, NP1EO, NP2EO, OP, and BPAare listed in Table
3
2.2 Other Publications:
1.
40 CFR Part 136,Appendix BDefinition and Procedure for
1.3 The values stated in SI units are to be regarded as
the Determination of the Method Detection Limit
standard. No other units of measurement are included in this
standard.
3. Terminology
1.4 This standard does not purport to address all of the
3.1 Definitions:
safety concerns, if any, associated with its use. It is the
3.1.1 For definitions of terms used in this standard, refer to
responsibility of the user of this standard to establish appro-
Terminology D1129.
priate safety, health, and environmental practices and deter-
3.2 Definitions of Terms Specific to This Standard:
mine the applicability of regulatory limitations prior to use.
3.2.1 bisphenol A, BPA, n—represents 4,4’-dihydroxy-2,2-
1.5 This international standard was developed in accor-
diphenylpropane.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
3.2.1.1 Discussion—Commercial bisphenol A is produced
Development of International Standards, Guides and Recom- by the condensation reaction of phenol and acetone to produce
mendations issued by the World Trade Organization Technical
predominantly the 4,4’-dihydroxy-2,2-diphenylpropane.
Barriers to Trade (TBT) Committee.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction ofASTM Committee D19 on Water contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor Standards volume information, refer to the standard’s Document Summary page on
Organic Substances in Water. the ASTM website.
3
Current edition approved Dec. 15, 2017. Published January 2018. Originally Available from U.S. Government Printing Office, Superintendent of
published in 2006. Last previous version approved in 2011 as D7065 – 11. DOI: Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
10.1520/D7065-17. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7065 − 17
TABLE 1 Method Detection Limit (MDL) and Reporting Limits
analyzed by GC/MS operated in the selected ion monitoring
A B
MDL, Reporting Range, (SIM) or full scan mode.
Analyte
(µg/L) (µg/L)
4.4 The target compounds are identified by retention time
NP 0.9 5.0–80.0
NP1EO 1.2 10.0–160.0 and confirmed by comparing the sample mass spectrum to that
NP2EO 1.8 20.0–320.0
of a known standard. The target compounds are quantitated
OP 0.2 1.0–16.0
using the quantitation ions of the target compounds utilizing
BPA 0.3 1.0–16.0
theinternalstandardsacenaphthene-d ,andphenanthrene-d .
A 10 10
MDL determined following th
...

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: D7065 − 11 D7065 − 17
Standard Test Method for
Determination of Nonylphenol, Bisphenol A, p-tert-
Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol
Diethoxylate in Environmental Waters by Gas
1
Chromatography Mass Spectrometry
This standard is issued under the fixed designation D7065; 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 determination of nonylphenol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol diethoxylate
(NP2EO), octylphenol (OP), and bisphenol A (BPA) that are partitioned into organic solvent, separated using gas chromatography
and detected with mass selective detection. These compounds or isomer mixtures are qualitatively and quantitatively determined
by this test method. This test method adheres to selected ion monitoring mass spectrometry but full scan mass spectrometry has
also been shown to work well under these conditions. Either analysis may be used.
1.2 The method detection limit (MDL) and reporting limit (RL) for NP, NP1EO, NP2EO, OP, and BPA are listed in Table 1.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 safety, health, and healthenvironmental practices and to determine the
applicability of regulatory limitations prior to use.
1.5 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
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
D5905 Practice for the Preparation of Substitute Wastewater
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3
2.2 Other Publications:
40 CFR Part 136, Appendix B Definition and Procedure for the Determination of the Method Detection Limit
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
3.2 Definitions:Definitions of Terms Specific to This Standard:
3.1.1 Nonylphenol, NP, n—nonylphenol is mixed isomers of branched p-nonylphenol.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved June 15, 2011Dec. 15, 2017. Published July 2011January 2018. Originally published in 2006. Last previous version approved in 20062011 as
D7065 – 06.11. DOI: 10.1520/D7065-11.10.1520/D7065-17.
2
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.
3
Available from U.S. Government Printing Office, Superintendent of Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7065 − 17
TABLE 1 MDL and Reporting Limits
3.1.1.1 Discussion—
A B
MDL Reporting Range
Analyte
, (μg/L) (μg/L)
NP 0.9 5.0-80.0
NP1EO 1.2 10.0-160.0
NP2EO 1.8 20.0-320.0
OP 0.2 1.0-16.0
BPA 0.3 1.0-16.0
TABLE 1 Method Detection Limit (MDL) and Reporting Limits
A B
MDL, Reporting Range,
Analyte
(μg/L) (μg/L)
NP 0.9 5.0–80.0
NP1EO 1.2 10.0–160.0
NP2EO 1.8 20.0–320.0
OP 0.2 1.0–16.0
BPA 0.3 1.0–16.0
A
MDL Determined Following Thedetermined following the Code of Federal
Regulations, 40 CFR Part 136, Appendix B.
B
Lowest Pointpoint of the Report
...