ASTM D7485-23

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

SIGNIFICANCE AND USE
5.1 NP and OP have been shown to have toxic effects in aquatic organisms. The source of NP and OP is prominently from the use of common commercial surfactants. The most widely used surfactant is nonylphenol ethoxylate (NPEO) which has an average ethoxylate chain length of nine. The ethoxylate chain is readily biodegraded to form NP1EO, NP2EO, nonylphenol carboxylate (NPEC) and, under anaerobic conditions, NP. NP will also biodegrade, but may be released into environmental waters directly at trace levels. This method has been investigated and is applicable for environmental waters, including seawater.
SCOPE
1.1 This test method covers the determination of nonylphenol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), and octylphenol (OP), extracted from water utilizing solid phase extraction (SPE), separated using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These compounds are qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.  
1.2 The method detection limit (MDL) and reporting limit (RL) for NP, NP1EO, NP2EO, and OP 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, 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-Apr-2023
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

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: D7485 − 23
Standard Test Method for
Determination of Nonylphenol, p-tert-Octylphenol,
Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate
in Environmental Waters by Liquid Chromatography/Tandem
1
Mass Spectrometry
This standard is issued under the fixed designation D7485; 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 D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of
1.1 This test method covers the determination of nonylphe-
Applicable Test Methods of Committee D19 on Water
nol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol di-
D3694 Practices for Preparation of Sample Containers and
ethoxylate (NP2EO), and octylphenol (OP), extracted from
for Preservation of Organic Constituents
water utilizing solid phase extraction (SPE), separated using
D3856 Guide for Management Systems in Laboratories
liquid chromatography (LC) and detected with tandem mass
Engaged in Analysis of Water
spectrometry (MS/MS). These compounds are qualitatively
D5847 Practice for Writing Quality Control Specifications
and quantitatively determined by this method. This method
for Standard Test Methods for Water Analysis
adheres to single reaction monitoring (SRM) mass spectrom-
D5905 Practice for the Preparation of Substitute Wastewater
etry.
3
2.2 Other Documents:
1.2 The method detection limit (MDL) and reporting limit
40 CFR Part 136, Appendix B Definition and Procedure for
(RL) for NP, NP1EO, NP2EO, and OP are listed in Table 1.
the Determination of the Method Detection Limit
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3. Terminology
standard.
3.1 Definitions:
1.4 This standard does not purport to address all of the
3.1.1 For definitions of terms used in this standard refer to
safety concerns, if any, associated with its use. It is the
Terminology D1129.
responsibility of the user of this standard to establish appro-
3.2 Definitions of Terms Specific to This Standard:
priate safety, health, and environmental practices and deter-
3.2.1 environmental water, n—shall refer to water tested
mine the applicability of regulatory limitations prior to use.
using this method; see Section 5.
1.5 This international standard was developed in accor-
3.2.2 nonylphenol, NP, n—is a mixture of branched
dance with internationally recognized principles on standard-
p-nonylphenol isomers; commercial NP is produced by the
ization established in the Decision on Principles for the
reaction of phenol with commercial nonene; commercial non-
Development of International Standards, Guides and Recom-
ene is not simply a linear C9H18 alpha olefin; it is a complex
mendations issued by the World Trade Organization Technical
mixture of predominantly nine-carbon olefins, called propylene
Barriers to Trade (TBT) Committee.
trimer, containing no linear isomers; this synthesis results in a
2. Referenced Documents
mixture of various branched nonylphenol isomers rather than a
2
discrete chemical structure; the branched nonyl group is
2.1 ASTM Standards:
positioned predominantly in the para position on the phenol
D1129 Terminology Relating to Water
ring.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
3.2.3 octylphenol, OP, n—commercial octylphenol is pro-
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
duced by the reaction of phenol and diisobutylene to produce
Organic Substances in Water.
predominantly the 4-(1,1,3,3-tetramethylbutyl)phenol isomer.
Current edition approved April 15, 2023. Published May 2023. Originally
approved in 2009. Last previous edition approved in 2016 as D7485 – 16. DOI:
10.1520/D7485-23.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Available from U.S. Government Printing Office Superintendent of Documents,
Standards volume information, refer to the standard’s Document Summary page on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
the ASTM website. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7485 − 23
TABLE 1 MDL and Reporting Limits
3.3.26 TC, n—Target Compound
A B
-6
MDL Reporting Range
Analyte 3.3.27 μM, n—
...

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: D7485 − 16 D7485 − 23
Standard Test Method for
Determination of Nonylphenol, p-tert-Octylphenol,
Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate
in Environmental Waters by Liquid Chromatography/Tandem
1
Mass Spectrometry
This standard is issued under the fixed designation D7485; 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 nonylphenol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol diethoxylate
(NP2EO), and octylphenol (OP), extracted from water utilizing solid phase extraction (SPE), separated using liquid chromatog-
raphy (LC) and detected with tandem mass spectrometry (MS/MS). These compounds are qualitatively and quantitatively
determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.
1.2 The method detection limit (MDL) and reporting limit (RL) for NP, NP1EO, NP2EO, and OP 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, 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on 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
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 Feb. 1, 2016April 15, 2023. Published March 2016May 2023. Originally approved in 2009. Last previous edition approved in 20092016 as
D7485D7485 – 16. – 09. DOI: 10.1520/D7485-16.DOI: 10.1520/D7485-23.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D7485 − 23
TABLE 1 MDL and Reporting Limits
A B
MDL Reporting Range
Analyte
(ng/L) (ng/L)
NP 33 100–2000
NP1EO 9 100–2000
NP2EO 9 100–2000
OP 24 100–2000
A
MDL Determined Followingdetermined following The Code of Federal
Regulations, 40 CFR Part 136, Appendix B.
B
Lowest Pointpoint of the Reporting Range is Calculatedreporting range is
calculated from the LV 1 Concentration Calibration Standardconcentration calibra-
tion standard in Table 4.
3
2.2 Other Documents:
The Code of Federal Regulations40 CFR Part 136, Appendix B 40 CFR Part 136, Appendix BDefinition 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 of Terms Specific to This Standard:
3.2.1 environmental water, n—shall refer to water tested using this method. Seemethod; see Section 5.
3.2.2 nonylphenol, NP, n—is a mixture of branched p-nonylphenol isomers. Commercialisomers; commercial NP is produced by
the reaction of phenol with commercial nonene. Commercialnonene; commercial nonene is not simply a linear C9H18 alpha olefin;
it is a complex mixture of predominantly nine-carbon olefins, called
...