ASTM D4657-92(1998)
(Test Method)Standard Test Method for Polynuclear Aromatic Hydrocarbons in Water (Withdrawn 2005)
Standard Test Method for Polynuclear Aromatic Hydrocarbons in Water (Withdrawn 2005)
SCOPE
1.1 This test method covers the determination of certain polynuclear aromatic hydrocarbons (PAHs) in water and wastewater. The following compounds may be determined by this test method: acenaphthene, acenaphthylene, anthracene, benzo(a)anthracene, benzo(a)pyrene, benzo(b)fluoranthene, benzo(ghi)perylene, benzo(k)fluoranthene, chrysene, dibenzo(ah)anthracene, fluoranthene, fluorene, indeno(1,2,3-cd)pyrene, naphthalene, phenathrene, and pyrene. Additional PAHs may also be determined; however, the analyst should demonstrate that the test method is in fact applicable to the specific PAH(s) of interest before applying it to sample analysis. This test method has high sensitivity for the compounds of interest. It is limited to use by analysts familiar with high-performance liquid chromatography (HPLC) or working under close supervision of such persons.
1.2 This test method is applicable to the determination of the compounds in 1.1 in water and wastewater. This test method has been successfully used with distilled water, tap water, surface water, and the following wastewaters: effluent from an oil refinery, blast furnace, and combined coke oven and blast furnace. It is the user's responsibility to ensure the validity of this test method for waters of untested matrices. It presupposes a high expectation of finding the specific compounds of interest. If the user is attempting to screen samples for any or all of the compounds above, component identities should be verified by using two different types of reverse phase HPLC columns, both ultraviolet and fluorescence detection, or gas chromatography/mass spectrometry-spectroscopy screening procedures, or both.
1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 9.
WITHDRAWN RATIONALE
This test method covers the determination of certain polynuclear aromatic hydrocarbons (PAHs) in water and wastewater. The following compounds may be determined by this test method: acenaphthene, acenaphthylene, anthracene, benzo(a)anthracene, benzo(a)pyrene, benzo(b)fluoranthene, benzo(ghi)perylene, benzo(k)fluoranthene, chrysene, dibenzo(ah)anthracene, fluoranthene, fluorene, indeno(1,2,3-cd)pyrene, naphthalene, phenathrene, and pyrene.
Formerly under the jurisdiction of Committee D19 on Water, this test method was withdrawn in January 2005. This standard is being withdrawn due to lack of use and lack of support to review and update the document.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation:D 4657–92 (Reapproved 1998)
Standard Test Method for
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Polynuclear Aromatic Hydrocarbons in Water
This standard is issued under the fixed designation D 4657; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method covers the determination of certain 2.1 ASTM Standards:
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polynuclear aromatic hydrocarbons (PAHs) in water and D 1129 Terminology Relating to Water
wastewater. The following compounds may be determined by D 1192 Specification for Equipment for Sampling Water
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this test method: acenaphthene, acenaphthylene, anthracene, and Steam in Closed Conduits
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benzo(a)anthracene, benzo(a)pyrene, benzo(b)fluoranthene, D 1193 Specification for Reagent Water
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benzo(ghi)perylene, benzo(k)fluoranthene, chrysene, diben- D 1253 Test Method for Residual Chlorine in Water
zo(ah)anthracene, fluoranthene, fluorene, indeno(1,2,3- D 3370 Practices for Sampling Water from Closed Con-
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cd)pyrene, naphthalene, phenathrene, and pyrene. Additional duits
PAHs may also be determined; however, the analyst should D 3856 Guide for Good Laboratory Practices in Laborato-
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demonstrate that the test method is in fact applicable to the ries Engaged in Sampling and Analysis of Water
specific PAH(s) of interest before applying it to sample D 4210 Practice for Intralaboratory Quality Control Proce-
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analysis. This test method has high sensitivity for the com- dures and a Discussion on Reporting Low-Level Data
pounds of interest. It is limited to use by analysts familiar with
3. Terminology
high-performance liquid chromatography (HPLC) or working
under close supervision of such persons. 3.1 Definitions—For definitions of terms used in this test
method, refer to Terminology D1129.
1.2 This test method is applicable to the determination of
the compounds in 1.1 in water and wastewater. This test
4. Summary of Test Method
method has been successfully used with distilled water, tap
4.1 This test method consists of the extraction of 1 L of
water, surface water, and the following wastewaters: effluent
water with methylene chloride. This extract is then reduced in
from an oil refinery, blast furnace, and combined coke oven
volume using Kuderna-Danish (K-D) evaporation followed by
and blast furnace. It is the user’s responsibility to ensure the
column chromatography on silica gel.The appropriate fraction
validity of this test method for waters of untested matrices. It
from the silica gel chromatography containing the PAHs is
presupposes a high expectation of finding the specific com-
again reduced in volume using K-D evaporation and is solvent
pounds of interest. If the user is attempting to screen samples
exchanged with acetonitrile to an exact volume of 1 mL. This
for any or all of the compounds above, component identities
concentrated extract is then analyzed for PAH using high-
shouldbeverifiedbyusingtwodifferenttypesofreversephase
performance liquid chromatography (HPLC).
HPLC columns, both ultraviolet and fluorescence detection, or
4.2 The HPLC analysis utilizes reverse phase chromatogra-
gas chromatography/mass spectrometry-spectroscopy screen-
phy using a combination of isocratic and gradient elution.
ing procedures, or both.
AcetonitrileandwaterareusedasthemobilephaseonaPerkin
1.3 This standard does not purport to address all of the
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Elmer PAH/10 reverse phase column. Other C-18 reverse
safety concerns, if any, associated with its use. It is the
phase columns may be used, provided that they yield adequate
responsibility of the user of this standard to establish appro-
resolution of the PAHs of interest. Fluorescence or ultraviolet
priate safety and health practices and determine the applica-
detection depending on the needs is used to monitor the PAH
bility of regulatory limitations prior to use. Specific hazards
of interest; quantitation is by peak area integration or peak
statements are given in Section 9.
height measurement. Results are reported in micrograms per
litre.
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This test method is under the jurisdiction ofASTM Committee D-19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
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Organic Substances in Water. Annual Book of ASTM Standards, Vol 11.01.
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Current edition approved Oct. 15, 1992. Published January 1993. Originally
Perkin-Elmer PAH/10 reverse phase column is available from Perkin-Elmer
published as D4657–87. Last previous edition D4657–91. Corporation, 761 Main Ave., Norwalk, CT 06859.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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