ASTM D6160-98
(Test Method)Standard Test Method for Determination of Polychlorinated Biphenyls (PCBs) in Waste Materials by Gas Chromatography
Standard Test Method for Determination of Polychlorinated Biphenyls (PCBs) in Waste Materials by Gas Chromatography
SCOPE
1.1 this test method is a two-tiered analytical approach to PCB screening and quantitation of liquid and solid wastes, such as oils, sludges, aqueous solutions, and other waste matrices.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 6160 – 98
Standard Test Method for
Determination of Polychlorinated Biphenyls (PCBs) in Waste
Materials by Gas Chromatography
This standard is issued under the fixed designation D 6160; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 1.7 Quantification limits will vary depending on the type of
waste stream being analyzed.
1.1 This test method is a two-tiered analytical approach to
1.8 This standard does not purport to address all of the
PCB screening and quantitation of liquid and solid wastes,
safety concerns, if any, associated with its use. It is the
such as oils, sludges, aqueous solutions, and other waste
responsibility of the user of this standard to establish appro-
matrices.
priate safety and health practices and determine the applica-
1.2 Tier I is designed to screen samples rapidly for the
bility of regulator limitations prior to use.
presence of PCBs.
1.3 Tier II is used to determine the concentration of PCBs,
2. Referenced Documents
typically in the range of from 2 to 50 mg/kg. PCB concentra-
2.1 ASTM Standards:
tions greater than 50 mg/kg are determined through analysis of
D 4059 Test Method for Analysis of Polychlorinated Biphe-
sample dilutions.
nyls in Insulating Liquids by Gas Chromatography
1.4 This is a pattern recognition approach, which does not
E 203 Test Method for Water Using Karl Fischer Reagent
take into account individual congeners that might occur, such
E 288 Specification for Laboratory Glass Volumetric
as in reaction by-products. This test method describes the use
3 Flasks
of Aroclors 1016, 1221, 1232, 1242, 1248, 1254, 1260, 1262,
E 355 Practice for Gas Chromatography Terms and Rela-
and 1268, as reference standards, but others could also be
tionships
included. Aroclors 1016 and 1242 have similar capillary gas
E 697 Practice for Use of Electron-capture Detectors in Gas
chromatography (GC) patterns. Interferences or weathering are
Chromatography
especially problematic with Aroclors 1016, 1232, and 1242 and
E 969 Specification for Glass Volumetric (Transfer) Pipet
may make distinction between the three difficult.
E 1510 Practice for Installing Fused Silica Open Tubular
NOTE 1—Aroclor is a registered trademark of Monsanto.
Capillary Columns in Gas Chromatography
1.5 This test method provides sample clean up and instru- 2.2 U.S. EPA Standards:
Method 608 Organochlorine Pesticides and PCBs Environ-
mental conditions necessary for the determination of Aroclors.
Gas chromatography (GC) using capillary column separation mental Monitoring and Support Laboratory, Cincinnati,
Ohio. EPA Report 600/4/82–057.
technique and electron capture detector (ECD) are described.
Other detectors, such as atomic emission detector (AED) and Method 680 Determination of Pesticides and PCBs in Water
mass spectrometry (MS), may be used if sufficient performance and Soil/Sediment by Gas Chromatography/Mass Spec-
trometry
(for example, sensitivity) is demonstrated. Further details about
the use of GC and ECD are provided in Practices E 355, E 697, Method 3620 Florisil Column Clean-Up
Method 3630 Silica Gel Clean-Up
and E 1510.
1.6 Quantitative results are reported on the dry weights of Method 3660 Sulfur Clean-Up
Method 8082 Determination of PCB in Water and Soil/
waste samples.
1 4
This test method is under the jurisdiction of ASTM Committee D02 on ASTM Annual Book of Standards, Vol. 10.03.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee ASTM Annual Book of Standards, Vol. 15.05.
D02.04 on Hydrocarbons Analysis. ASTM Annual Book of Standards, Vol. 14.02.
Current edition approved Nov. 10, 1998. Published January 1999. Originally EPA Report 600/4/82–057. “Organochlorine Pesticides and PCBs” Environ-
published as D 6160 – 97. Last previous edition D 6160 – 97. mental Monitoring and Support Laboratory, Cincinnati, OH.
2 8
This test method is based largely on EPA 8080 (and the proposed modification “Determination of Pesticides and PCBs in Water and Soil/Sediment by Gas
for the use of capillary columns, EPA 8081) and EPA Report 600/4–81–045 by Chromatography/Mass Spectrometry”, Ann Alford-Stevens et al, Physical and
Bellar, T. and J. Lichtenberg, reported in 1981. The report is titled,“ The Chemical Methods Branch, Environmental Monitoring and Support Laboratory
Determination of Polychlorinated Biphenyls in Transformer Fluid and Waste Oils” Office of Research and Development, USEPA, Cincinnati, OH 45268.
and provides significant support to the protocol below. U.S. EPA, “Test Methods for Evaluating Solid Waste, Physical/Chemical
Aroclor Standards may be purchased as 1000 ug/mL in isooctane. Methods,” SW-846.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 6160 – 98
Sediment by Gas Chromatography: Capillary Column checked with a standard concentration of 0.01 ug/mL (each)
Technique and for higher level work (10 ppm), the instrument is checked
with a 0.1 ug/mL standard.
3. Terminology
4.3 Identification involves a pattern comparison of the
3.1 Definitions of Terms Specific to This Standard:
chromatograms of an unknown sample with that of a standard
3.1.1 Aroclors, n—commercial mixtures of polychlorinated
obtained under identical instrumental conditions.
biphenyl congeners marketed and trademarked by Monsanto
4.4 When quantification is required (Tier II), an external
prior to 1977.
standards method (ESTD) is used. The quantitation technique
3.1.1.1 Discussion—Specific Aroclors are usually desig-
typically requires a comparison of five peaks (minimum of
nated by a four-digit number, with the first two digits usually
three) between the chromatograms of an unknown sample and
designating the number of carbon atoms and the last two digits
that of standard Aroclor obtained under identical conditions.
providing the chlorine content (for example, Aroclor 1260 is 60
Quantitation of either Aroclors 1016 or 1260 is performed
% (weight) chlorine).
using a five-point calibration of a mixed Aroclor standard
3.1.2 congeners, n—compounds related by structural simi-
containing Aroclors 1016 and 1260. All remaining Aroclors are
larities.
quantitated from single point calibrations. Calibration is veri-
3.1.2.1 Discussion—All polychlorinated biphenyls (PCBs)
fied daily by comparison of results obtained for analysis of the
share the same C structure and vary only by the number and
12 midpoint calibration standard of Aroclar 1016 and 1260 to the
position of the chlorine atoms attached to the aromatic rings.
five-point calibration curve. (See Appendix X1 for an example
3.1.3 continuing calibration standard (CCS)—a known
chromatogram and calibration table.)
blend or one or more Aroclors at a fixed concentration that is
5. Significance and Use
injected into the gas chromatograph to demonstrate the validity
of the calibration.
5.1 This test method provides sufficient PCB data for many
3.1.4 dry weight, n—concentration of PCBs after factoring
regulatory requirements. While the most common regulatory
out the water content.
level is 50 ppm (dry weight corrected), lower limits are used in
3.1.4.1 Discussion—This correction assumes that all PCBs
some locations. Since sensitivities will vary for different types
originated from nonaqueous sources and any water present has
of samples, one shall demonstrate a sufficient method detection
been added subsequently, diluting the original concentration.
limit for the matrix of interest.
This correction can be described using the formula:
5.2 This test method differs from Test Method D 4059 in
that it provides for more sample clean-up options, utilizes a
Aroclor ~mg/Kg!~wet!
Aroclor ~mg/Kg!~dry!5 (1)
capillary column for better pattern recognition and interference
~100 2 % water!/100
discrimination, and includes both a qualitative screening and a
3.1.5 instrument performance standard (IPS), n—a known
quantitative results option.
low level of an Aroclor in a clean solvent used as a comparator
to determine which qualitative (screening) results are of
6. Interferences
sufficient magnitude to require quantitative analyses.
6.1 The ECD has selective sensitivity to alkyl halides,
3.1.6 surrogate,n, n—compound or compounds that are
conjugated carbonyls, nitrogen compounds, organometallics,
similar to analytes of interest in chemical composition, extrac-
and sulfur. Therefore, the chromatogram obtained for each
tion, and chroatography, but that are not normally found at
sample shall be carefully compared to chromatograms of
significant levels in the matrices of interest.
standards to allow proper interpretation.
3.1.6.1 Discussion—Surrogates may be spiked into blanks,
6.2 Solvents, reagents, glassware, and other sample process-
standards, samples, or matrix spikes prior to analysis to allow
ing hardware may yield artifacts or interferences, or both, to
a determination of a quantitative recovery rate. Surrogates are
standard analysis. All these materials shall be demonstrated to
also used to document matrix effects and method control.
be free from interferences under the conditions of analysis by
3.1.7 waste material, n—any matter, within the scope of this
analyzing method blanks.
test method, that is in the process of being recycled or
6.3 Interferences from phthalate esters may pose a major
disposed.
problem in Aroclor determinations when using ECD. Phtha-
lates generally appear in the chromatogram as broad late
4. Summary of Test Method
eluting peaks. Since phthalates are commonly used as plasti-
4.1 The sample is extracted with solvent and the extract is
cizers and are easily extracted from plastic, all contact of
treated to remove interfering substances, if needed. The sample
samples and extracts with plastic should be avoided.
extract is injected into a gas chromatograph. The components
6.4 While general clean-up techniques are provided as part
are separated as they pass through the capillary column and
of this test method, some samples may require additional
polychlorinated biphenyl compounds, if present, are detected
clean-up beyond the scope of this test method before proper
by an ECD.
instrumental analysis may be performed.
NOTE 2—Portions of this test method are similar to EPA Methods 608,
680, and 8082. 7. Apparatus
4.2 For screening (Tier I), instrument performance is moni- 7.1 Gas Chromatograph, a temperature programmable gas
tored by a 2-uL injection of a standard containing Aroclors chromatograph suitable for splitless injections; equipped with
1016 and 1260. For low level work (1 ppm) the instrument is an ECD.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 6160 – 98
7.2 Data System, a data system capable of measuring peak 8.4 Hexane—See Note 4.
areas.
NOTE 4—Warning: Extremely flammable. Harmful if inhaled. May
7.3 Regulator (Make-up Gas)—N or Ar:Methane (95:5);
produce nerve cell damage. Vapors may cause flash fire.
two stage regulator rated at 20 MPa (3000 psi) inlet and 35 to
8.5 Isooctane—See Note 5.
860 kPa (5 to 125 psi) outlet.
7.4 Regulator (Carrier Gas)—H , two-stage regulator rated
NOTE 5—Warning: Extremely flammable. Harmful if inhaled. Vapors
at 20 MPa (3000 psi) inlet and 35 to 860 kPa (5 to 125 psi)
may cause flash fire.
outlet.
8.6 Methanol—See Note 6.
7.5 Gas Purifiers, to remove moisture and particulates.
Depending on the levels and types of interferences encoun-
NOTE 6—Warning: Flammable. Vapor harmful. May be fatal or cause
tered, these might involve molecular sieves (moisture), acti- blindness if swallowed or inhaled. Cannot be made nonpoisonous.
vated carbon (organics), or other commercially-available me-
8.7 Silynization Reagent (for example, 5 % dimethyldichlo-
dia.
rosilane in toluene). See Annex A2 for instructions.
7.6 Flow Meter, to measure gas flow. Typical range is from
8.8 Sodium Sulfate, granular, anhydrous (maintained at
0.5 to 50 mL/min. 6 0.1 mL/min.
130°C for at least 24 h prior to use). Cool the sodium sulfate in
7.7 Column, crosslinked 5 % phenyl methyl silicone, 30 m
a desiccator for 30 min before use.
by 0.32 mm id by 0.25 um film thickness.
8.9 Sulfuric Acid (concentrated):
7.7.1 It is possible that other columns will provide sufficient
8.10 Acetone/Hexane, 10 % acetone/90 % hexane (v/v).
separating power, but this shall be demonstrated before use.
8.11 Gases, Hydrogen (zero grade; 99.995 % purity) and
7.8 Analytical Balance, capable of weighing to 0.0001 g.
nitrogen (zero grade; 99.998 % purity) or argon/methane (95:5;
7.9 Volumetric Flasks, 10, 50, 100, 200 mL, (see Specifica-
ECD grade).
tion E 288) Class A with ground-glass stoppers.
8.11.1 Care shall be given to ensure purity of the carrier gas.
7.10 Vortex Mixer:
For example, an in-line filter may be required.
7.11 Vials, glass, 20 mL and 40 mL capacity with TFE-
8.12 Aroclor Standards , Aroclor 1016, 1221, 1232, 1242,
fluorocarbon-lined caps.
1254, 1260, 1262, 1268.
7.12 Septum Inserts— Inserts shall be treated with a si-
8.13 Decachlorobiphenyl (DCB) (surrogate) Optional:
lynization reagent before use or after cleaning. (See Annex A2
8.13.1 Surrogate Stock Standard (15 ug/mL) Preparation—
for possible procedure.) They may be purchased already
Accurately dilute 1.5 mL of 1000 ug/mL DCB concentrate in
treated.
100 mL volumetric flask and fill to the mark with methanol,
7.13 Volumetric Pipette, 1, 5, 10 mL (see Specification E
yielding a 15 ug/mL solution.
969), Class A.
8.13.2 Surrogate Working Standard (1.5 ug/mL)
7.14 Syringe, 500 uL, mechanical guide.
Preparation—Accurately dilute 10 mL of the 15 ug/mL DCB
8. Reagents and Materials
stock standard in a 100 mL volumetric flask and fill to the mark
8.1 Purity of Reagents—Reagent grade chemicals shall be
with methanol, yielding a 1.5 ug/mL working DCB standard.
used in all tests. Unless otherwise indicated, it is intended that
NOTE 7—Sample preparations will normally use 0.1 mL of this solu-
all reagents conform to the specifications of the Committee on
tion. The resulting concentration in the sample extract is 0.005 ug/mL
Analytical Reagents of the American Chemical Society where
before any further dilutions. The following calculations show this.
such specifications are available. Other grades may be
...
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