ASTM D6160 - 21 (2025) 用气相色谱法测定废料中多氯联苯（PCBs）的标准试验方法

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Designation: D6160 −21 (Reapproved 2025)
Standard Test Method for
Determination of Polychlorinated Biphenyls (PCBs) in Waste
Materials by Gas Chromatography
1
This standard is issued under the ﬁxed designation D6160; 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
2
covers a two-tiered analytical ap-
proach to PCB screening and quantitation of liquid and solid
wastes, such as oils, sludges, aqueous solutions, and other
waste matrices.
1.2 Tier I is designed to screen samples rapidly for the
presence of PCBs.
1.3 Tier II is used to determine the concentration of PCBs,
typically in the range of from 2 mg ⁄kg to 50 mg ⁄kg. PCB
concentrations greater than 50 mg/kg are determined through
analysis of sample dilutions.
1.4 This is a pattern recognition approach, which does not
take into account individual congeners that might occur, such
as in reaction by-products. This test method describes the use
of Aroclors
3
1016, 1221, 1232, 1242, 1248, 1254, 1260, 1262,
and 1268, as reference standards, but others could also be
included. Aroclors 1016 and 1242 have similar capillary gas
chromatography (GC) patterns. Interferences or weathering are
especially problematic with Aroclors 1016, 1232, and 1242 and
may make distinction between the three difficult.
1.5 This test method provides sample clean up and instru-
mental conditions necessary for the determination of Aroclors.
Gas chromatography (GC) using capillary column separation
technique and electron capture detector (ECD) are described.
Other detectors, such as atomic emission detector (AED) and
mass spectrometry (MS), may be used if sufficient performance
(for example, sensitivity) is demonstrated. Further details about
the use of GC and ECD are provided in Practices E355,E697,
and E1510.
1.6 Quantitative results are reported on the dry weights of
waste samples.
1.7 Quantiﬁcation limits will vary depending on the type of
waste stream being analyzed.
1.8 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
standard.
1.9 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 appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.10 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
4
D4059 Test Method for Analysis of Polychlorinated Biphe-
nyls in Insulating Liquids by Gas Chromatography
D4175 Terminology Relating to Petroleum Products, Liquid
Fuels, and Lubricants
E203 Test Method for Water Using Volumetric Karl Fischer
Titration
E288 Speciﬁcation for Laboratory Glass Volumetric Flasks
E355 Practice for Gas Chromatography Terms and Relation-
ships
E697 Practice for Use of Electron-Capture Detectors in Gas
Chromatography
E969 Speciﬁcation for Glass Volumetric (Transfer) Pipets
E1510 Practice for Installing Fused Silica Open Tubular
Capillary Columns in Gas Chromatographs
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.04.0L on Gas Chromatography Methods.
Current edition approved Oct. 1, 2025. Published October 2025. Originally
approved in 1997. Last previous edition approved in 2021 as D6160 – 21. DOI:
10.1520/D6160-21R25.
2
This test method is based largely on EPA 8080 (and the proposed modiﬁcation
for the use of capillary columns, EPA 8081) and EPA Report 600/4–81–045 by
Bellar, T. and J. Lichtenberg, reported in 1981. The report is titled, “The
Determination of Polychlorinated Biphenyls in Transformer Fluid and Waste Oils,”
and provides signiﬁcant support to the protocol in this standard.
3
Aroclor Standards may be purchased as 1000 µg/mL in isooctane. Aroclor is a
registered trademark of the Monsanto Company, 800 N. Lindbergh Blvd., St. Louis,
MO 63167.
4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at www.astm.org/contact. 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
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.
1

2.2 U.S. EPA Standards:

Method 608 Organochlorine Pesticides and PCBs

Method 680 Determination of Pesticides and PCBs in Water

and Soil/Sediment by Gas Chromatography/Mass Spec-

trometry

Method 3620 Florisil Column Clean-Up

Method 3630 Silica Gel Clean-Up

Method 3660 Sulfur Clean-Up

Method 8082 Determination of PCB in Water and Soil/

Sediment by Gas Chromatography: Capillary Column

Technique

3. Terminology

3.1 Deﬁnitions:

3.1.1 This test method makes reference to common gas

chromatographic procedures, terms, and relationships. Detailed

deﬁnitions of these can be found in Practice E355 and

Terminology D4175. In addition, deﬁnition of terms speciﬁc to

this standard include:

3.1.2 Aroclors, n—commercial mixtures of polychlorinated

biphenyl congeners marketed and trademarked by Monsanto

prior to 1977.

3.1.2.1 Discussion—Speciﬁc Aroclors are usually desig-

nated by a four-digit number, with the ﬁrst two digits usually

designating the number of carbon atoms and the last two digits

providing the chlorine content (for example, Aroclor 1260 is

60 % (weight) chlorine).

3.1.3 congeners, n—compounds related by structural simi-

larities.

3.1.3.1 Discussion—All polychlorinated biphenyls (PCBs)

share the same C

structure and vary only by the number and

position of the chlorine atoms attached to the aromatic rings.

3.1.4 continuing calibration standard (CCS)—a known

blend or one or more Aroclors at a ﬁxed concentration that is

injected into the gas chromatograph to demonstrate the validity

of the calibration.

3.1.5 dry weight, n—concentration of PCBs after factoring

out the water content.

3.1.5.1 Discussion—This correction assumes that all PCBs

originated from nonaqueous sources and any water present has

been added subsequently, diluting the original concentration.

This correction can be described using the formula:

Aroclor

mg/Kg

! ~

dry

5Aroclor

mg/Kg

! ~

wet

100 2% water

/100 (1)

3.1.6 instrument performance standard (IPS), n—a known

low level of an Aroclor in a clean solvent used as a comparator

to determine which qualitative (screening) results are of

sufficient magnitude to require quantitative analyses.

3.1.7 surrogate, n—compound or compounds that are simi-

lar to analytes of interest in chemical composition, extraction,

and chromatography, but that are not normally found at

signiﬁcant levels in the matrices of interest.

3.1.7.1 Discussion—Surrogates may be spiked into blanks,

standards, samples, or matrix spikes prior to analysis to allow

a determination of a quantitative recovery rate. Surrogates are

also used to document matrix effects and method control.

3.1.8 waste material, n—any matter, within the scope of this

test method, that is in the process of being recycled or

disposed.

4. Summary of Test Method

4.1 The sample is extracted with solvent and the extract is

treated to remove interfering substances, if needed. The sample

extract is injected into a gas chromatograph. The components

are separated as they pass through the capillary column and

polychlorinated biphenyl compounds, if present, are detected

by an ECD.

NOTE 1—Portions of this test method are similar to EPA Methods 608,

680, and 8082.

4.2 For screening (Tier I), instrument performance is moni-

tored by a 2 µL injection of a standard containing Aroclors

1016 and 1260. For low level work (1 ppm) the instrument is

checked with a standard concentration of 0.01 µg ⁄mL (each)

and for higher level work (10 ppm), the instrument is checked

with a 0.1 µg ⁄mL standard.

4.3 Identiﬁcation involves a pattern comparison of the

chromatograms of an unknown sample with that of a standard

obtained under identical instrumental conditions.

4.4 When quantiﬁcation is required (Tier II), an external

standards method (ESTD) is used. The quantitation technique

typically requires a comparison of ﬁve peaks (minimum of

three) between the chromatograms of an unknown sample and

that of standard Aroclor obtained under identical conditions.

Quantitation of either Aroclors 1016 or 1260 is performed

using a ﬁve-point calibration of a mixed Aroclor standard

containing Aroclors 1016 and 1260. All remaining Aroclors are

quantitated from single point calibrations. Calibration is veri-

ﬁed daily by comparison of results obtained for analysis of the

midpoint calibration standard of Aroclor 1016 and 1260 to the

ﬁve-point calibration curve. (See Appendix X1 for an example

chromatogram and calibration table.)

5. Signiﬁcance and Use

5.1 This test method provides sufficient PCB data for many

regulatory requirements. While the most common regulatory

level is 50 ppm (dry weight corrected), lower limits are used in

some locations. Since sensitivities will vary for different types

of samples, one shall demonstrate a sufficient method detection

limit for the matrix of interest.

5.2 This test method differs from Test Method D4059 in that

it provides for more sample clean-up options, utilizes a

capillary column for better pattern recognition and interference

discrimination, and includes both a qualitative screening and a

quantitative results option.

6. Interferences

6.1 The ECD has selective sensitivity to alkyl halides,

conjugated carbonyls, nitrogen compounds, organometallics,

EPA Report 600/4/82–057, Environmental Monitoring and Support Laboratory,

Cincinnati, OH.

Alford-Stevens, Ann, et al, Physical and Chemical Methods Branch, Environ-

mental Monitoring and Support Laboratory Office of Research and Development,

USEPA, Cincinnati, OH.

U.S. EPA, “Test Methods for Evaluating Solid Waste,” Physical/Chemical

Methods, SW-846.

D6160 − 21 (2025)

and sulfur. Therefore, the chromatogram obtained for each

sample shall be carefully compared to chromatograms of

standards to allow proper interpretation.

6.2 Solvents, reagents, glassware, and other sample process-

ing hardware may yield artifacts or interferences, or both, to

standard analysis. All these materials shall be demonstrated to

be free from interferences under the conditions of analysis by

analyzing method blanks.

6.3 Interferences from phthalate esters may pose a major

problem in Aroclor determinations when using ECD. Phtha-

lates generally appear in the chromatogram as broad late

eluting peaks. Since phthalates are commonly used as plasti-

cizers and are easily extracted from plastic, all contact of

samples and extracts with plastic should be avoided.

6.4 While general clean-up techniques are provided as part

of this test method, some samples may require additional

clean-up beyond the scope of this test method before proper

instrumental analysis may be performed.

7. Apparatus

7.1 Gas Chromatograph, a temperature programmable gas

chromatograph suitable for splitless injections; equipped with

an ECD.

7.2 Data System, a data system capable of measuring peak

areas.

7.3 Regulator (Make-up Gas)—N

or Ar:Methane (95:5);

two stage regulator rated at 20 MPa (3000 psi) inlet and 35 kPa

to 860 kPa (5 psi to 125 psi) outlet.

7.4 Regulator (Carrier Gas)—H

, two-stage regulator rated

at 20 MPa (3000 psi) inlet and 35 kPa to 860 kPa (5 psi to

125 psi) outlet.

7.5 Gas Puriﬁers, to remove moisture and particulates.

Depending on the levels and types of interferences

encountered, these might involve molecular sieves (moisture),

activated carbon (organics), or other commercially-available

media.

7.6 Flow Meter, to measure gas ﬂow. Typical range is from

0.5 mL ⁄min. to 50 mL ⁄min. 60.1 mL ⁄min.

7.7 Column, crosslinked 5 % phenyl methyl silicone, 30 m

by 0.32 mm id by 0.25 µm ﬁlm thickness.

7.7.1 It is possible that other columns will provide sufficient

separating power, but this shall be demonstrated before use.

7.8 Analytical Balance, capable of weighing to 0.0001 g.

7.9 Volumetric Flasks, 10 mL, 50 mL, 100 mL, 200 mL,

(see Speciﬁcation E288) Class A with ground-glass stoppers.

7.10 Vortex Mixer:

7.11 Vials, glass, 20 mL and 40 mL capacity with TFE-

ﬂuorocarbon-lined caps.

7.12 Septum Inserts—Inserts shall be treated with a silyni-

zation reagent before use or after cleaning. (See Annex A2 for

possible procedure.) They may be purchased already treated.

7.13 Volumetric Pipette, 1 mL, 5 mL, 10 mL (see Speciﬁ-

cation E969), Class A.

7.14 Syringe, 500 µL, mechanical guide.

8. Reagents and Materials

8.1 Purity of Reagents—Reagent grade chemicals shall be

used in all tests. Unless otherwise indicated, it is intended that

all reagents 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.

8.2 Acetone—(Warning—Extremely ﬂammable. Vapors

may cause ﬂash ﬁre.)

8.3 Activated Magnesium Silicate (Florisil), Pesticide resi-

due (PR) grade (60/100 mesh); store in glass containers with

ground glass stoppers or foil lined screw caps.

8.3.1 Just before use, activate each batch at least 4 h at

130 °C in a glass container loosely covered with aluminum

foil. Alternatively, store the magnesium silicate in an oven at

130 °C. Cool the magnesium silicate in a desiccator for 30 min

before use.

8.4 Hexane—(Warning—Extremely ﬂammable. Harmful if

inhaled. May produce nerve cell damage. Vapors may cause

ﬂash ﬁre.)

8.5 Isooctane—(Warning—Extremely ﬂammable. Harmful

if inhaled. Vapors may cause ﬂash ﬁre.)

8.6 Methanol—(Warning—Flammable. Vapor harmful.

May be fatal or cause blindness if swallowed or inhaled.

Cannot be made nonpoisonous.)

8.7 Silynization Reagent (for example, 5 % dimethyldichlo-

rosilane in toluene). See Annex A2 for instructions.

8.8 Sodium Sulfate, granular, anhydrous (maintained at

130 °C for at least 24 h prior to use). Cool the sodium sulfate

in a desiccator for 30 min before use.

8.9 Sulfuric Acid (concentrated):

8.10 Acetone/Hexane, 10 % acetone/90 % hexane (v/v).

8.11 Gases, Hydrogen (zero grade; 99.995 % purity) and

nitrogen (zero grade; 99.998 % purity) or argon/methane (95:5;

ECD grade).

8.11.1 Care shall be given to ensure purity of the carrier gas.

For example, an in-line ﬁlter may be required.

8.12 Aroclor Standards

, Aroclor 1016, 1221, 1232, 1242,

1254, 1260, 1262, 1268.

8.13 Decachlorobiphenyl (DCB) (surrogate) Optional:

8.13.1 Surrogate Stock Standard (15 µg/mL) Preparation—

Accurately dilute 1.5 mL of 1000 µg ⁄mL DCB concentrate in

100 mL volumetric ﬂask and ﬁll to the mark with methanol,

yielding a 15 µg ⁄mL solution.

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. Pharma-

copeial Convention, Inc. (USPC), Rockville, MD.

D6160 − 21 (2025)

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标签： #标准试验 #试验方法 #标准试验方法

摘要：

本篇文章针对ASTM D6160 - 21 (2025)标准，详细阐述了如何利用气相色谱法（GC）准确测定废料中多氯联苯（PCBs）的含量。该标准为废料处理、环境监测及合规检验提供了权威的试验流程与质量控制要求。文章深入解析了方法原理、样品前处理步骤、色谱条件设置及数据判定准则，帮助实验室技术人员与环保从业者快速掌握PCBs定量分析的关键技术要点，从而提升检测结果的可靠性与法规符合性。

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ASTM D6160 - 21 (2025) 用气相色谱法测定废料中多氯联苯（PCBs）的标准试验方法

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