ASTM D7065-11
(Test Method)Standard Test Method for Determination of Nonylphenol, Bisphenol A, p-tert -Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters by Gas Chromatography Mass Spectrometry
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 Nonylphenol3, 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 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.4 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.5 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 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 method. This 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.TABLE 1 MDL and Reporting Limits
Analyte
MDLA, (μg/L)
Reporting RangeB (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 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 and health practices and to determine the applicability of regulatory limitations prior to use.
General Information
Relations
Buy Standard
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D7065 − 11
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 Engaged in Analysis of Water
D5847Practice for Writing Quality Control Specifications
1.1 This test method covers determination of nonylphenol
for Standard Test Methods for Water Analysis
(NP), nonylphenol ethoxylate (NP1EO), nonylphenol di-
D5905Practice for the Preparation of SubstituteWastewater
ethoxylate(NP2EO),octylphenol(OP),andbisphenolA(BPA)
E691Practice for Conducting an Interlaboratory Study to
that are partitioned into organic solvent, separated using gas
Determine the Precision of a Test Method
chromatography and detected with mass selective detection.
These compounds or isomer mixtures are qualitatively and
3. Terminology
quantitativelydeterminedbythismethod.Thismethodadheres
to selected ion monitoring mass spectrometry but full scan 3.1 Definitions:
mass spectrometry has also been shown to work well under
3.1.1 Nonylphenol, NP, n—nonylphenol is mixed isomers
these conditions. Either analysis may be used.
of branched p-nonylphenol.
3.1.1.1 Discussion—Commercial nonylphenol is produced
1.2 The method detection limit (MDL) and reporting limit
by the reaction of phenol with commercial nonene. Commer-
(RL) for NP, NP1EO, NP2EO, OP, and BPAare listed in Table
cial nonene is not simply a linear C H alpha olefin; it is a
1. 9 18
complex mixture of predominantly nine-carbon olefins, called
1.3 The values stated in SI units are to be regarded as
propylene trimer, containing no linear isomers. This synthesis
standard. No other units of measurement are included in this
results in a mixture of various branched nonylphenol isomers
standard.
rather than a discrete chemical structure. The branched nonyl
1.4 This standard does not purport to address all of the
group is positioned predominantly in the para position on the
safety concerns, if any, associated with its use. It is the
phenol ring.
responsibility of the user of this standard to establish appro-
3.1.2 Octylphenol, OP, n—OP represents 4-(1,1,3,3-
priate safety and health practices and to determine the
tetramethylbutyl)phenol.
applicability of regulatory limitations prior to use.
3.1.2.1 Discussion—Commercial octylphenol is produced
by the reaction of phenol and diisobutylene to produce pre-
2. Referenced Documents
dominantly the 4-(1,1,3,3-tetramethylbutyl)phenol isomer.
2
2.1 ASTM Standards:
3.1.3 Bisphenol A, BPA, n-BPA represents 4,4’-dihydroxy-
D1193Specification for Reagent Water
2,2-diphenylpropane.
D3694Practices for Preparation of Sample Containers and
3.1.3.1 Discussion—Commercial bisphenol A is produced
for Preservation of Organic Constituents
by the condensation reaction of phenol and acetone to produce
D3856Guide for Management Systems in Laboratories
predominantly the 4,4’-dihydroxy-2,2-diphenylpropane.
3.1.4 Environmental water, n—it shall refer to water tested
1 using this method. See Section 5.
This test method is under the jurisdiction ofASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor 3.2 Abbreviations:
Organic Substances in Water.
3.2.1 NP1EO—branched nonylphenol monoethoxylate.
Current edition approved June 15, 2011. Published July 2011. Originally
3.2.2 NP2EO—branched nonylphenol diethoxylate.
published in 2006. Last previous version approved in 2006 as D7065 – 06. DOI:
10.1520/D7065-11.
3.2.3 n-NP—normal straight chain nonylphenol.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.2.3.1 Discussion—n-NP is used in this method as a
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
surrogate for NP, OPand BPA. n-NPis not produced commer-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. ciallyandisnotexpectedtobefoundinenvironmentalwaters.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D7065 − 11
TABLE 1 MDL and Reporting Limits
samples and is applicable to these matrices. It has not been
A B
Analyte MDL , (µg/L) Reporting Range (µg/L) investigated for use with salt water or solid sample matrices.
NP 0.9 5.0-80.0
5.2 The first reported synthesis of BPAwas by the reaction
NP1EO 1.2 10.0-160.0
4
NP2EO 1.8 20.0-320.0
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D7065–06 Designation: D7065 – 11
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 bisphenolA(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 method. This 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) 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 and health practices and to determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
D3856 Guide for Good Laboratory Practices in Laboratories Engaged in Sampling and 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. Terminology
3.1 NPrepresents nonylphenol which is mixed isomers of branched p-nonylphenol. Commercial nonylphenol (NP) is produced
by the reaction of phenol with commercial nonene. Commercial nonene is not simply a linear C H alpha olefin; it is a complex
9 18
mixture of predominantly nine-carbon olefins, called propylene trimer, containing no linear isomers. This synthesis results in a
mixtureofvariousbranchednonylphenolisomersratherthanadiscretechemicalstructure.Thebranchednonylgroupispositioned
predominantly in the para position on the phenol ring.
3.2 OP represents octylphenol. Commercial octylphenol is produced by the reaction of phenol and diisobutylene to produce
predominantly the 4-(1,1,3,3-tetramethylbutyl)phenol isomer.
3.3 BPA represents bisphenol A. Commercial bisphenol A is produced by the condensation reaction of phenol and acetone to
produce predominantly the 4,48-isopropylidenediphenol isomer.
3.4 NP1EO represents branched nonylphenol monoethoxylate.
3.5 NP2EO represents branched nonylphenol diethoxylate.
3.6 n-NPand n-NP1EO represent normal straight chain nonylphenol and nonylphenol ethoxylate. n-NPand n-NP1EO are used
in this method as surrogates. They are not produced commercially and are not expected to be found in environmental waters.
3.7 Environmental water shall refer to water tested using this method. See Section 5.
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 Dec. 15, 2006. Published January 2007. DOI: 10.1520/D7065-06.
Current edition approved June 15, 2011. Published July 2011. Originally published 2006. Last previous version approved 2006 as D7065–06.DOI: 10.1520/D7065-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. 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 ----------------------
D7065 – 11
TABLE 1 MDL and Reporting Limits
Analyte MDL, (µg/L) Reportin
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.