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: D6160 − 98 (Reapproved 2017)

Standard Test Method for

Determination of Polychlorinated Biphenyls (PCBs) in Waste
Materials by Gas Chromatography1
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 1.6 Quantitative results are reported on the dry weights of

2
1.1 This test method covers a two-tiered analytical ap- waste samples.
proach to PCB screening and quantitation of liquid and solid 1.7 Quantification limits will vary depending on the type of
wastes, such as oils, sludges, aqueous solutions, and other waste stream being analyzed.
waste matrices. 1.8 The values stated in SI units are to be regarded as
1.2 Tier I is designed to screen samples rapidly for the standard. No other units of measurement are included in this
presence of PCBs. standard.
1.3 Tier II is used to determine the concentration of PCBs, 1.9 This standard does not purport to address all of the
typically in the range of from 2 mg ⁄kg to 50 mg ⁄kg. PCB safety concerns, if any, associated with its use. It is the
concentrations greater than 50 mg/kg are determined through responsibility of the user of this standard to establish appro-
analysis of sample dilutions. priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.4 This is a pattern recognition approach, which does not
1.10 This international standard was developed in accor-
take into account individual congeners that might occur, such
dance with internationally recognized principles on standard-
as in reaction by-products. This test method describes the use
ization established in the Decision on Principles for the
of Aroclors3 1016, 1221, 1232, 1242, 1248, 1254, 1260, 1262,
Development of International Standards, Guides and Recom-
and 1268, as reference standards, but others could also be
mendations issued by the World Trade Organization Technical
included. Aroclors 1016 and 1242 have similar capillary gas
Barriers to Trade (TBT) Committee.
chromatography (GC) patterns. Interferences or weathering are
especially problematic with Aroclors 1016, 1232, and 1242 and 2. Referenced Documents
may make distinction between the three difficult.
2.1 ASTM Standards:4
1.5 This test method provides sample clean up and instru- D4059 Test Method for Analysis of Polychlorinated Biphe-
mental conditions necessary for the determination of Aroclors. nyls in Insulating Liquids by Gas Chromatography
Gas chromatography (GC) using capillary column separation E203 Test Method for Water Using Volumetric Karl Fischer
technique and electron capture detector (ECD) are described. Titration
Other detectors, such as atomic emission detector (AED) and E288 Specification for Laboratory Glass Volumetric Flasks
mass spectrometry (MS), may be used if sufficient performance E355 Practice for Gas Chromatography Terms and Relation-
(for example, sensitivity) is demonstrated. Further details about ships
the use of GC and ECD are provided in Practices E355, E697, E697 Practice for Use of Electron-Capture Detectors in Gas
and E1510. Chromatography
1
E969 Specification for Glass Volumetric (Transfer) Pipets
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
E1510 Practice for Installing Fused Silica Open Tubular
Subcommittee D02.04.0L on Gas Chromatography Methods. Capillary Columns in Gas Chromatographs
Current edition approved Oct. 1, 2017. Published November 2017. Originally 2.2 U.S. EPA Standards:
approved in 1997. Last previous edition approved in 2013 as D6160 – 98 (2013).
DOI: 10.1520/D6160-98R17.
Method 608 Organochlorine Pesticides and PCBs5
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
4
Bellar, T. and J. Lichtenberg, reported in 1981. The report is titled, “The For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Determination of Polychlorinated Biphenyls in Transformer Fluid and Waste Oils,” contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
and provides significant support to the protocol in this standard. Standards volume information, refer to the standard’s Document Summary page on
3
Aroclor Standards may be purchased as 1000 µg/mL in isooctane. Aroclor is a the ASTM website.
5
registered trademark of the Monsanto Company, 800 N. Lindbergh Blvd., St. Louis, EPA Report 600/4/82–057, Environmental Monitoring and Support Laboratory,
MO 63167. Cincinnati, OH.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 D6160 − 98 (2017)
Method 680 Determination of Pesticides and PCBs in Water 4. Summary of Test Method
and Soil/Sediment by Gas Chromatography/Mass Spec- 4.1 The sample is extracted with solvent and the extract is
trometry6 treated to remove interfering substances, if needed. The sample
Method 3620 Florisil Column Clean-Up7 extract is injected into a gas chromatograph. The components
Method 3630 Silica Gel Clean-Up7 are separated as they pass through the capillary column and
Method 3660 Sulfur Clean-Up7 polychlorinated biphenyl compounds, if present, are detected
Method 8082 Determination of PCB in Water and Soil/ by an ECD.
Sediment by Gas Chromatography: Capillary Column
Technique7 NOTE 1—Portions of this test method are similar to EPA Methods 608,
680, and 8082.
3. Terminology 4.2 For screening (Tier I), instrument performance is moni-
3.1 Definitions of Terms Specific to This Standard: tored by a 2 µL injection of a standard containing Aroclors
3.1.1 Aroclors, n—commercial mixtures of polychlorinated 1016 and 1260. For low level work (1 ppm) the instrument is
biphenyl congeners marketed and trademarked by Monsanto checked with a standard concentration of 0.01 µg ⁄mL (each)
prior to 1977. and for higher level work (10 ppm), the instrument is checked
3.1.1.1 Discussion—Specific Aroclors are usually desig- with a 0.1 µg ⁄mL standard.
nated by a four-digit number, with the first two digits usually 4.3 Identification involves a pattern comparison of the
designating the number of carbon atoms and the last two digits chromatograms of an unknown sample with that of a standard
providing the chlorine content (for example, Aroclor 1260 is obtained under identical instrumental conditions.
60 % (weight) chlorine).
4.4 When quantification is required (Tier II), an external
3.1.2 congeners, n—compounds related by structural simi- standards method (ESTD) is used. The quantitation technique
larities. typically requires a comparison of five peaks (minimum of
3.1.2.1 Discussion—All polychlorinated biphenyls (PCBs) three) between the chromatograms of an unknown sample and
share the same C12 structure and vary only by the number and that of standard Aroclor obtained under identical conditions.
position of the chlorine atoms attached to the aromatic rings. Quantitation of either Aroclors 1016 or 1260 is performed
3.1.3 continuing calibration standard (CCS)—a known using a five-point calibration of a mixed Aroclor standard
blend or one or more Aroclors at a fixed concentration that is containing Aroclors 1016 and 1260. All remaining Aroclors are
injected into the gas chromatograph to demonstrate the validity quantitated from single point calibrations. Calibration is veri-
of the calibration. fied daily by comparison of results obtained for analysis of the
3.1.4 dry weight, n—concentration of PCBs after factoring midpoint calibration standard of Aroclor 1016 and 1260 to the
out the water content. five-point calibration curve. (See Appendix X1 for an example
3.1.4.1 Discussion—This correction assumes that all PCBs chromatogram and calibration table.)
originated from nonaqueous sources and any water present has
been added subsequently, diluting the original concentration. 5. Significance and Use
This correction can be described using the formula: 5.1 This test method provides sufficient PCB data for many
Aroclor ~ mg/Kg! ~ wet! regulatory requirements. While the most common regulatory
Aroclor ~ mg/Kg! ~ dry! 5 (1)
~ 100 2 % water! /100 level is 50 ppm (dry weight corrected), lower limits are used in
3.1.5 instrument performance standard (IPS), n—a known some locations. Since sensitivities will vary for different types
low level of an Aroclor in a clean solvent used as a comparator of samples, one shall demonstrate a sufficient method detection
to determine which qualitative (screening) results are of limit for the matrix of interest.
sufficient magnitude to require quantitative analyses. 5.2 This test method differs from Test Method D4059 in that
3.1.6 surrogate, n—compound or compounds that are simi- it provides for more sample clean-up options, utilizes a
lar to analytes of interest in chemical composition, extraction, capillary column for better pattern recognition and interference
and chromatography, but that are not normally found at discrimination, and includes both a qualitative screening and a
significant levels in the matrices of interest. quantitative results option.
3.1.6.1 Discussion—Surrogates may be spiked into blanks,
standards, samples, or matrix spikes prior to analysis to allow 6. Interferences
a determination of a quantitative recovery rate. Surrogates are 6.1 The ECD has selective sensitivity to alkyl halides,
also used to document matrix effects and method control. conjugated carbonyls, nitrogen compounds, organometallics,
3.1.7 waste material, n—any matter, within the scope of this and sulfur. Therefore, the chromatogram obtained for each
test method, that is in the process of being recycled or sample shall be carefully compared to chromatograms of
disposed. standards to allow proper interpretation.
6.2 Solvents, reagents, glassware, and other sample process-
6
Alford-Stevens, Ann, et al, Physical and Chemical Methods Branch, Environ- ing hardware may yield artifacts or interferences, or both, to
mental Monitoring and Support Laboratory Office of Research and Development,
standard analysis. All these materials shall be demonstrated to
USEPA, Cincinnati, OH.
7
U.S. EPA, “Test Methods for Evaluating Solid Waste,” Physical/Chemical be free from interferences under the conditions of analysis by
Methods, SW-846. analyzing method blanks.

2
 D6160 − 98 (2017)
6.3 Interferences from phthalate esters may pose a major such specifications are available.8 Other grades may be used,
problem in Aroclor determinations when using ECD. Phtha- provided it is first ascertained that the reagent is of sufficiently
lates generally appear in the chromatogram as broad late high purity to permit its use without lessening the accuracy of
eluting peaks. Since phthalates are commonly used as plasti- the determination.
cizers and are easily extracted from plastic, all contact of 8.2 Acetone—(Warning—Extremely flammable. Vapors
samples and extracts with plastic should be avoided. may cause flash fire.)
6.4 While general clean-up techniques are provided as part 8.3 Activated Magnesium Silicate (Florisil), Pesticide resi-
of this test method, some samples may require additional due (PR) grade (60/100 mesh); store in glass containers with
clean-up beyond the scope of this test method before proper ground glass stoppers or foil lined screw caps.
instrumental analysis may be performed. 8.3.1 Just before use, activate each batch at least 4 h at
130 °C in a glass container loosely covered with aluminum
7. Apparatus foil. Alternatively, store the magnesium silicate in an oven at
7.1 Gas Chromatograph, a temperature programmable gas 130 °C. Cool the magnesium silicate in a desiccator for 30 min
chromatograph suitable for splitless injections; equipped with before use.
an ECD. 8.4 Hexane—(Warning—Extremely flammable. Harmful if
7.2 Data System, a data system capable of measuring peak inhaled. May produce nerve cell damage. Vapors may cause
areas. flash fire.)
7.3 Regulator (Make-up Gas)—N2 or Ar:Methane (95:5); 8.5 Isooctane—(Warning—Extremely flammable. Harmful
two stage regulator rated at 20 MPa (3000 psi) inlet and 35 to if inhaled. Vapors may cause flash fire.)
860 kPa (5 to 125 psi) outlet. 8.6 Methanol—(Warning—Flammable. Vapor harmful.
7.4 Regulator (Carrier Gas)—H2, two-stage regulator rated May be fatal or cause blindness if swallowed or inhaled.
at 20 MPa (3000 psi) inlet and 35 to 860 kPa (5 to 125 psi) Cannot be made nonpoisonous.)
outlet. 8.7 Silynization Reagent (for example, 5 % dimethyldichlo-
rosilane in toluene). See Annex A2 for instructions.
7.5 Gas Purifiers, to remove moisture and particulates.
Depending on the levels and types of interferences 8.8 Sodium Sulfate, granular, anhydrous (maintained at
encountered, these might involve molecular sieves (moisture), 130 °C for at least 24 h prior to use). Cool the sodium sulfate
activated carbon (organics), or other commercially-available in a desiccator for 30 min before use.
media. 8.9 Sulfuric Acid (concentrated):
7.6 Flow Meter, to measure gas flow. Typical range is from 8.10 Acetone/Hexane, 10 % acetone/90 % hexane (v/v).
0.5 mL ⁄min. to 50 mL ⁄min. 6 0.1 mL ⁄min.
8.11 Gases, Hydrogen (zero grade; 99.995 % purity) and
7.7 Column, crosslinked 5 % phenyl methyl silicone, 30 m nitrogen (zero grade; 99.998 % purity) or argon/methane (95:5;
by 0.32 mm id by 0.25 µm film thickness. ECD grade).
7.7.1 It is possible that other columns will provide sufficient 8.11.1 Care shall be given to ensure purity of the carrier gas.
separating power, but this shall be demonstrated before use. For example, an in-line filter may be required.
7.8 Analytical Balance, capable of weighing to 0.0001 g. 8.12 Aroclor Standards3, Aroclor 1016, 1221, 1232, 1242,
1254, 1260, 1262, 1268.
7.9 Volumetric Flasks, 10 mL, 50 mL, 100 mL, 200 mL,
(see Specification E288) Class A with ground-glass stoppers. 8.13 Decachlorobiphenyl (DCB) (surrogate) Optional:
8.13.1 Surrogate Stock Standard (15 µg/mL) Preparation—
7.10 Vortex Mixer:
Accurately dilute 1.5 mL of 1000 µg ⁄mL DCB concentrate in
7.11 Vials, glass, 20 mL and 40 mL capacity with TFE- 100 mL volumetric flask and fill to the mark with methanol,
fluorocarbon-lined caps. yielding a 15 µg ⁄mL solution.
7.12 Septum Inserts—Inserts shall be treated with a silyni- 8.13.2 Surrogate Working Standard (1.5 µg ⁄mL)
zation reagent before use or after cleaning. (See Annex A2 for Preparation—Accurately dilute 10 mL of the 15 µg ⁄mL DCB
possible procedure.) They may be purchased already treated. stock standard in a 100 mL volumetric flask and fill to the mark
with methanol, yielding a 1.5 µg ⁄mL working DCB standard.
7.13 Volumetric Pipette, 1 mL, 5 mL, 10 mL (see Specifi-
cation E969), Class A. NOTE 2—Sample preparations will normally use 0.1 mL of this solu-
tion. The resulting concentration in the sample extract is 0.005 µg ⁄mL
7.14 Syringe, 500 µL, mechanical guide. before any further dilutions. The following calculations show this.

8. Reagents and Materials 8

Reagent Chemicals, American Chemical Society Specifications, American
8.1 Purity of Reagents—Reagent grade chemicals shall be Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
used in all tests. Unless otherwise indicated, it is intended that
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
all reagents conform to the specifications of the Committee on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Analytical Reagents of the American Chemical Society where MD.

3
 D6160 − 98 (2017)
1.5 µg/mL 3 0.l mL 5 0.15 µg (2) 8.15.1 Calibration Check Standard (CCS) (Tier
2–Quantitation)—This standard contains 0.1 µg ⁄mL (those
0.15 µg who are interested in the 20 mg ⁄Kg level with no compositing,
5 0.005 µg/mL
~ 3.0 mL sample127 mL! use 0.2 µg ⁄mL each) each of Aroclors 1016 and 1260 in
8.14 Calibration Standards: hexane.
8.14.1 Intermediate Stock Standard (50 µg ⁄mL): If high 8.15.1.1 The surrogate concentration, if used, is
level standards (for example, commercially available standards 0.005 µg ⁄mL.
at 2000 µg ⁄mL to 5000 µg/mL) have been purchased, prepare 8.15.1.2 Example—To prepare the CCS along with DCB,
solutions of 50 µg ⁄mL concentration. add 20 mL of Aroclors 1016/1260 to 0.5 µg ⁄mL and 0.05 mL
8.14.1.1 The surrogate calibration standard may be added of DCB at 10 µg ⁄mL into 100 mL volumetric flask. Dilute to
(optional) to the Aroclor 1016/1260 intermediate stock stan- 100 mL volume with isooctane. Mix well. This yields a
dard at a concentration of 2.5 µg ⁄mL. For preparation of the 0.1 µg ⁄mL of CSS and 0.005 µg ⁄mL of DCB.
standard, add 500 µL of 50 µg ⁄mL surrogate to a 10 mL 8.15.2 Matrix Spiking Standard (Tier 2–Quantitation)—The
volumetric flask containing 3.0 mL of isooctane. Add the matrix spiking standard is to contain Aroclor 1268 at a
Aroclor 1016/1260 standard (5.0 mL at 100 µg ⁄mL) to the concentration of 50 µg ⁄mL in methanol. Laboratories working
flask. Dilute to 10 mL volume with isooctane and mix well. at lower calibration ranges will need to dilute this (for example,
8.14.1.2 To prepare the continuing CCS, dilute 200 µL of to 25 µg ⁄mL).
the intermediate stock standard to 100 mL. 8.16 Copper Powder, 200 mesh, 99 % min.
Volume add into Ar-1016/1260 concentration Surrogate concentration
the 100 mL flask µg/mL µg/mL
8.17 Silica Gel, 100 to 200 mesh.
200 µL 0.10 0.005
9. Sampling
8.14.2 Instrument Performance Standard (IPS) (Tier 9.1 PCBs are hydrophobic compounds. Therefore, when
I–Screening)—An isooctane solution of Aroclors 1016 and sampling, all organic phases, including bottom sludge beneath
1260 is prepared at a concentration of 0.01 µg ⁄mL (each) or aqueous phases, shall be sampled. Given the possible presence
0.1 µg ⁄mL (each) (depending on whether the minimum level of of alcohols and glycols, it is typically not acceptable to sample
interest is 2 µg ⁄mL or 20 µg ⁄mL) from the appropriate stock the organic phase only.
standard.
8.14.2.1 If the surrogate (decachlorobiphenyl, (DCB)) is 9.2 Headspace above stored standards and samples or ex-
used, it shall be added to the IPS to result in a concentration of tracts should be minimized such that the volume is less than
0.005 µg ⁄mL. 50 %.
8.14.2.2 To prepare the IPS along with DCB, add 10 mL of 9.3 Three mL of sample are required for each determination.
Aroclor 1016/1260 at 0.1 µg ⁄mL and 0.033 mL of DCB at No special sample preservation is required other than storage in
15 µg ⁄mL into 100 mL volumetric flask. Dilute to 100 mL a closed container with minimal headspace. It is accepted
volume with isooctane. Mix well. This yields 0.01 µg ⁄mL IPS practice to use borosilicate glass containers with TFE-
and 0.005 µg ⁄mL of DCB. fluorocarbon-lined lids.
8.14.2.3 The following additional standards shall be run
10. Preparation of Apparatus
once (at 0.1 µg ⁄mL) to demonstrate the Aroclor patterns and be
mixed if preferred. 10.1 General Gas Chromatographic Conditions—The first
temperature profile (12 min run time) is used for Tier I
Aroclor Mix with the following:
1268 1221 or 1232 or 1242 or 1248 or 1254 screening method for the presence of Aroclor. The longer
1262 1221 or 1232 or 1242 or 1248 second temperature profile (17 min run time) is used for Tier II
1254 1221
to quantitate the Aroclors present, but may also be used for Tier
8.14.3 Individual Working Standards (Tier I, if desired.
2–Quantitation)—Working standards are typically prepared in 10.1.1 Rapid Screen Capillary Column Oven Temperature
isooctane at concentrations of 0.02 µg ⁄mL, 0.05 µg ⁄mL, Profile (Tier I, 12 min run time):
0.1 µg ⁄mL, 0.3 µg ⁄mL and 0.5 µg ⁄mL for Aroclors 1016 and Initial value 130 °C
1260. All other Aroclors are prepared at the mid level concen- Initial time 2 min
tration (0.1 µg ⁄mL) for the single point calibration. An alter- Program rate 20 °C ⁄min
Final value 270 °C
native calibration range may be used as long as the criteria for Final time 3 min
linearity of the calibration range is documented. Carrier gas hydrogen
8.14.3.1 Aroclors 1016 and 1260 shall be a mixed standard. Head pressure depend on DCB RT
(approximately 105 KPa (15 psi)) column
The following additional standards shall be run once (at flow: 3.1 mL ⁄min-3.2 mL ⁄min
0.1 µg ⁄mL) to demonstrate the Aroclor patterns and may be Make-up gas nitrogen or argon: methane
mixed, if preferred. Make-up gas rate approximately 65 mL ⁄min.
Splitless mode
Aroclor May be mixed with: Purge off 0 min
Purge on 1.0 min
1268 1221 or 1232 or 1242 or 1248 or 1254 Purge vent 2.5 mL/min
1262 1221 or 1232 or 1242 or 1248 Split vent 50 mL/min
1254 1221 Sample injection 2.0 µL
Injector inlet system 250 °C
8.15 Quality Control Standards: Detector 315 °C

4
 D6160 − 98 (2017)
10.1.2 Quantitation Capillary Column Oven Temperature 11.1.2.1 Tabulate the sum of the areas or the data system
Profile (Tier II, 17 min run time; may also be used for Tier I calculated amount of the five major peaks for each of the
analysis: Aroclors 1016 and 1260 in the instrument performance stan-
Initial value 125 °C dard. The response shall be within 50 % of the initial response.
Initial time 3 min Initial response shall be established by averaging the response
Level I
of a minimum of five injections of the instrument performance
Program rate 12 °C ⁄min standard (IPS). If the limit is exceeded, new limits may need to
Final value 270 °C be established.
Final time 2 min
11.1.2.2 Likewise, the expected response for the surrogate,
Carrier gas hydrogen if used, is established by averaging the areas of DCB in the five
Head pressure Depend on DCB RT initial IPS analyses.
(approximately, 105 KPa (15 psi))
Column flow 3.1 mL/min (approximately at 270 °C) 11.1.2.3 The surrogate also may be used for retention time
Make-up gas nitrogen control. It is recommended that column flow be adjusted so
Make-up gas rate approximately 65 mL/min
DCB elutes between 10.5 min to 11.5 min using the 12 min GC
Splitless mode program. (This will typically require a column head pressure of
Purge off 0 min 105 kPa to 112 kPa.) (Alternatively, the retention time should
Purge on 1.0 min
Purge rate 50 mL/min
be 15 min to 16.5 min using the 17 min program.)
Sample injection 2.0 µL 11.1.3 Tier 2–Quantitative Method—The GC data system
must be calibrated for both Aroclors 1016 and 1260, using five
Injector inlet system 250 °C
Detector 315 °C peaks for each Aroclor. [For example, when using an
integrator, divide the standard amount by the number of peaks
11. Calibration and Standardization being used. Using five peaks on a 0.5 µg ⁄mL standard would
assign 0.1 µg ⁄mL to each peak. This will allow for a calibration
11.1 Calibration:
table to be made, yielding response factors for each peak at the
11.1.1 Tier 1–Screening Method—Aroclors are multi-peak
five levels of calibration. Set up a calibration table in the
chemical mixtures that have very unique identification pat-
method file of the integrator or data system that is to be used.
terns. All Aroclors shall be run individually or in mixtures at
Calculate an average response factor for each of five peaks for
0.1 µg ⁄mL on each channel performing screening to produce
both Aroclors. Calculate the standard deviation of the average
reference patterns. It is important to note that some of these
response factor for each peak of the Aroclor using the
patterns have the same constituents and that some Aroclors are
following calculation.
quantitated using the same peaks (such as Aroclors 1016 and
1232 or 1242). When screening for Aroclors, a visual determi-
nation is made by the following key items: S5 Œ( n

i51
~Xi 2 X!2
n21
(3)
11.1.1.1 Aroclor pattern—(a) same singlets, doublets, and
triplets present in the reference chromatograms, and (b) same where:
relative peak heights between peaks in the sample chromato- S = standard deviation,
gram and the reference chromatogram. Xi = each observed value,
11.1.1.2 Retention time shifts should be very consistent X = the arithmetic mean of observed values, and
between the standard and the sample peaks. n = total number of calibration points.
11.1.1.3 All samples in which an Aroclor is detected (using 11.1.3.1 Calculate the percent relative standard deviations
Tier I) require a judgment concerning the amount. The recog- (% RSDs) for the response factors of the calibrated peaks for
nized Aroclor pattern shall be compared to the IPS each Aroclor from the formula below. The acceptance criteria
(0.01 µg ⁄mL or 0.1 µg ⁄mL). If the overall level of the sus- for the % RSD for each Aroclor is ≤20 %. If the average %
pected Aroclor pattern is equal to or greater than overall level RSD is greater than 20 % for either Aroclor, then linearity over
of the IPS pattern, then Tier II analysis may be used to the desired calibration range for that instrument has not been
quantitate the sample. If multiple Aroclors are suspected, a Tier demonstrated.
II analysis may be run to help resolve the mixture.
11.1.1.4 Recovery control limits for the surrogate are 40 % NOTE 3—The % RSD is 100 % multiplied by the result of Eq 3 (s)
divided by the arithmetic mean (X ).
to 150 % recovered. If the recovery is outside of these limits,
see Annex A1. 11.1.3.2 When samples are to be analyzed, instrument
11.1.2 Tier I Calibration Check—An instrument perfor- control is verified by analyzing the CCS and the percent
mance standard (IPS) at 0.01 µg ⁄mL of Aroclor 1016 and 1260 difference (% D) is calculated. The acceptance criteria is
is used to check the instrument sensitivity once a day or every within +30 % for each AROCLOR in the CCS (1016 and
20 samples, whichever is more frequent (typically laboratories 1260).
using ten samples compositing shall use the 0.01 µg ⁄mL 11.1.3.3 If either Aroclor 1016 or 1260 is out of control for
standard to achieve a detection limit of 5 µg ⁄mL of Aroclor in the daily CCS, corrective action shall be taken and a CCS
any individual sample). Sample results will be compared reanalyzed. If corrective action does not correct the problem,
qualitatively with the daily IPS. (See the Calculation section then a new five point calibration curve shall be created.
13). Percent difference (% D)

5
 D6160 − 98 (2017)
AmtI 2 Amt C 11.2.5 Matrix Spike Duplicate (MSD) Sample (Tier II
%D5 3 100 % (4) only)—Every batch or 20 samples, whichever is more frequent,
AmtI
precision data is generated using a matrix spike duplicate.
where:
Acceptance criteria is 20 % relative percent difference (RPD)
AmtI = amount in standard, and for the duplicate analyses.
AmtC = calculated amount from current CCS.
11.2.5.1 RPD is calculated from the absolute difference
11.1.3.4 Calibration for Aroclors other than Aroclor 1016 between duplicate percent recovery results D1 and D2 divided
and Aroclor 1260 will be performed by analyzing standards at by the mean value of the duplicates.
the concentration representing the midpoint of the calibration
range selected. For example, if calibration is desired over the RPD 5
?D 1 2 D2 ? 3 100 % (6)
~ D 1 1D 2 ! /2
range of 0.02 µg ⁄mL to 0.5 µg ⁄mL, then the 0.1 µg ⁄mL stan-
dards shall be used for calibration. Therefore, a five point 12. Procedure
calibration shall be performed for Aroclors 1016 and 1260 and
a one-point calibration shall be performed for all remaining 12.1 Compositing—It is common to analyze mixtures of
Aroclors. multiple samples, called composites, if a large number of
11.1.3.5 After the linearity of the system has been samples are analyzed. This approach is described in Annex A3.
demonstrated, and each of the remaining Aroclors has been 12.2 Sample Preparation Procedure:
analyzed using middle level concentration, recalibration will
12.2.1 Liquid Samples—Accurately pipette 3.0 mL of
be required only when the calibration check standard criteria is
sample into a tared 40 mL vial (fitted with a TFE-fluorocarbon-
met. Old calibration curves may not be used again, other than
lined cap) and weight. If the results are calculated by weight
to review data generated using those calibration curves.
accurately weigh the sample and record the weight. Spike this
11.2 Standardization: sample with 100 µL of decachlorobiphenyl surrogate working
11.2.1 Surrogate Recovery—Recovery control limits for the standard.
surrogate are 40 % to 150 % recovered. 12.2.1.1 Add 27 mL acetone/hexane to the vial, producing a
11.2.1.1 If the recovery is outside of these limits, see Annex 1:10 dilution. Cap it and vortex vigorously for at least 30 s. If
A1. the sample is not completely miscible with acetone/hexane,
11.2.2 Method Blank—For every 20 samples or batch, add more acetone to reach a total of approximately 30 mL
whichever is more frequent, a method blank shall be prepared extract and vortex again. (Alternatively, place capped vial in
by processing the extraction solvent (with surrogate, if used) sonic bath for 5 min.)
through the same clean-up as that used for the samples. This is 12.2.2 Solid, Semi-solids, Sludge Samples—Weigh accu-
to detect possible contamination picked up during the sample rately 3.0 g of sample into a 40 mL vial fitted with a TFE-
clean-up process. fluorocarbon-lined cap. Spike this sample with 100 µL of
NOTE 4—A batch is the group of samples prepared at the same time. A decachlorobiphenyl surrogate working standard. Add 30 mL of
batch may not exceed 20 samples. acetone/hexane to the vial for a 1:10 dilution. Vortex for at least
11.2.3 Calibration Check Standard (CCS) (Tier II only)—A 30 s.
0.1 µg ⁄mL standard (or 0.2 µg ⁄mL) obtained from a source 12.2.2.1 If the sample does not totally dissolve, vortex again
separate from the intermediate standard and containing Aro- or place capped vial in sonic bath for 5 min. This shall provide
clors 1016 and 1260 is the CCS which is used to verify the adequate contact whether or not any further dissolution occurs.
validity of the five-point calibration curve. The calculated 12.2.3 Matrix Spike and Matrix Spike Duplicate Samples—
results for the CCS shall agree with the current calibration Add 1.0 mL of spiking solution to the sample just after the
curve to within 630 % percent difference (% D). If the CCS addition of the surrogate and prior to the addition of the
results indicate that the calibration is outside control limits, and acetone-hexane solvent.
routine maintenance does not correct the problem, then the 12.2.4 Centrifuge—If sediment is visible, centrifuge the
GC/ECD must be recalibrated. extract to separate out the sediment.
11.2.4 Matrix Spike (MS) Samples (Tier II only)—For every
12.3 Sample Clean-up—Clean-up is not required for all
batch or 20 samples, whichever is more frequent, a sample
samples; however, interference problems due to the presence of
requiring Tier II analysis shall be selected in an unbiased
other chemical species may usually be addressed using the
manner and spiked with Aroclor 1268. These results shall be
procedures found in Annex A4.
documented, with an example shown in Appendix X2.
11.2.4.1 1.0 mL of 50 µg ⁄mL of Aroclor 1268 (25 µg ⁄mL, if 12.4 Gas Chromatographic Analysis Sequence—Samples
working at lower calibration range) is added to the sample are analyzed in a set referred to as an analysis sequence.
chosen for spiking. Matrix spiked sample recovery limits are 12.4.1 Tier 1–Screening:
from 60 % to 140 %, providing any Aroclor present in the 12.4.1.1 Standards Sequence (initially and optionally with
sample before spiking does not exceed five times the spike recalibrations)—(a) Aroclor 1016/1260, at selected IPS level
level. (5 times) and (b) The following may be mixed as described
Recovered amount below and shall be analyzed at 0.1 µg ⁄mL each (for 20 mg ⁄Kg
% Recovery 5 3 100 % (5)
Spiked amount level of interest use 0.2 µg ⁄mL).

6
 D6160 − 98 (2017)

Aroclor 1221 is equal to or greater than the overall level of the IPS pattern,
Aroclor 1232 then Tier II analysis may be used to quantitate the PCBs.
Aroclor 1242
Aroclor 1248
13.1.3 If Aroclor identification is prevented by the presence
Aroclor 1254 of interferences, additional sample preparation is required. All
Aroclor 1262 composites having such interferences shall be analyzed as
Aroclor 1268
individual samples. Individual samples may be diluted prior to
12.4.1.2 Some of the standards in 12.4.1.1 may be run as analysis, but it must be remembered that the detection limit of
mixed standards: the analysis has been changed. Used oil samples shall not be
Aroclor May be Mixed With diluted beyond 1:100 during initial screening analysis to meet
the regulated level of interest (2 µg ⁄mL).
1268 1221 or 1232 or 1242 or 1248 or 1254
1262 1221 or 1232 or 1242 or 1248 13.1.4 If PCBs are detected, (when compared to the IPS
1254 1221 criteria above) the result is reported Positive. If no PCBs are
12.4.1.3 A Typical Analysis Sequence—A typical analysis detected above the IPS level, the result is Negative.
sequence includes (a) reagent blank (optional), (b) Instrument 13.1.5 When screening for Aroclors, visual determination is
Performance Standard (IPS) (every 20 samples or every day, made by the following key items:
whichever is more frequent), (c) method blank, and (d) 13.1.5.1 Aroclor Pattern—The Aroclor pattern includes (a)
Samples 1 to 20. Same singlets, doublets, and triplets present in the reference
12.4.1.4 Repeat this sequence as long as the system meets chromatograms, and (b) Same relative peak heights between
the IPS criteria. peaks in the sample chromatogram and the reference chromato-
gram.
12.4.2 Tier 2–Quantitation:
13.1.5.2 Retention times shall be very consistent between
12.4.2.1 Standards Sequence—The standards sequence in- the standard and the sample peaks.
cludes (a) reagent blank, (b) Aroclor 1016/1260 (5 point
calibration), (c) Aroclor 1268 mid-level standard, (d) Mid level 13.2 Data System Quantitation—The GC data system shall
standard of suspected Aroclors if not, 1016 or 1260, and (e) be calibrated for each Aroclor using a minimum of five peaks
(CCS, five times, to establish DCB response, if DCB is not (with exception of Aroclor 1221, which uses three peaks) for
spiked in 1016/1260 standards.) each Aroclor. For use with integrators, divide the standard
12.4.2.2 A Typical Analysis Sequence—A typical analysis amount by the number of peaks being used (for example, using
sequence includes (a) reagent blank (optional), (b) CCS (1016/ five peaks on a 0.5 µg ⁄mL standard would assign 0.1 µg ⁄mL to
1260 mid standard), (c) method blank, (d) Samples 1 to 20, (e) each peak.) For some data systems, the total standard amount
matrix spike sample, and (f) matrix spike duplicate. may be assigned to each peak. This will allow for a calibration
table to be made, yielding response factors for each peak.
12.4.2.3 Repeat this sequence as long as the system meets
the quality assurance criteria. NOTE 5—Response factors are based on amount/area for some data
systems, while response factors are based on area/amount for others.
12.5 Inject 2 µL of the sample extract into the gas chromato-
graph using an autosampler or a manual injection. 13.2.1 Quantitation of Aroclor in samples requires selecting
five peaks that are free of interferences (minimum of three
12.6 Set the data display (printer or video screen) conditions peaks, if interferences present) in the TIER II analysis, and
so that a mid point calibration standard shall be full scale on the assigning the appropriate response factor to each peak.
chromatogram. 13.2.2 Aroclors 1016/1260 are quantitated using a five point
12.7 If the results exceed the calibrated range of the system, calibration. All other Aroclors use a single point calibration.
and quantitation is desired, the extract shall be diluted and Samples exceeding the working range shall be diluted prior to
reanalyzed within the calibration range. analysis so that quantitation is performed within the calibration
range.
13. Calculation 13.2.3 As an example, the data system shall be set up to
provide results in µg/mL. The following equation yields the
13.1 Screening—Aroclors are made up of numerous conge- concentration of Aroclors in mg/kg on a wet weight basis.
ners and so the chromatograms are multi-peak. Often the
Aroclor ~ µg/mL! 3 dilution volume 10 mL
chromatogram of the sample may not exactly match that of the Aroclor ~ mg/kg! ~ wet! 5 3
sample wt ~ g ! 1 mL
standard due to factors such as environmental exposure,
interferences not easily removed by cleanup techniques, and (7)
the presence of multiple Aroclors. After determining the water content, using Test Method
13.1.1 Visual determinations are made by comparing the E203, the concentration of Aroclor in a sample is corrected for
chromatogram with the reference chromatograms. Set the data dry weight of the sample by the following:
display conditions so that a 0.1 µg ⁄mL standard is full scale on Aroclor g/kg ~ wet!
the chromatogram. Aroclor mg/kg ~ dry! 5 (8)
~ 100 2 % water! /100
13.1.2 All samples in which an Aroclor is detected require a
judgment concerning the amount. The recognized Aroclor Water content is usually determined by Test Method E203.
pattern shall be compared to the IPS (0.01 µg ⁄mL or 13.3 Manual Quantitation—Quantitate Aroclor samples by
0.1 µg ⁄mL). If the overall level of the suspected Aroclor pattern comparing the area of five sample peaks (minimum of three, if

7
 D6160 − 98 (2017)
interferences present) to the area of the same peaks from Aroclors to combine to produce the appropriate reference
appropriate (mid level) reference standards. Use only those material. A calibration standard is then made using this blend.
peaks from the sample that are attributed to Aroclors. These Use only those peaks from the sample that are attributed to
peaks shall be present in the chromatogram of reference chlorobiphenyls. These peaks shall be present in the reference
materials. See Aroclor Calculation Work Sheet (Appendix X2.) blend.
for an example of how to perform manual quantitation.
14. Precision and Bias9
13.3.1 Use the following formulas to calculate the concen-
tration of each of the Aroclor peaks in the sample (wet weight): 14.1 The precision of this test method was determined by
statistical examination of interlaboratory study results. All data
Aroclor ~ wet! Peak No. 1 ~ µg/mL! 5 (9)
was generated using GC/ECD.
sample area 3 dilution volume ~ mL! NOTE 7—Ten samples in the range of 4.3 mg ⁄kg to 61.4 mg/kg PCBs
standard area 3 sample volume ~ mL! with water content in the range 0 % to 72 % were analyzed in duplicate at
ten different laboratories using ten operators.
dilution volume No. 1 14.1.1 Repeatability—The difference between two results
3 ~ standard concentrate µg/mL! 3
aliquot volume obtained by the same operator with the same apparatus under
13.3.2 This is repeated for each peak used, and the results constant operating conditions on identical test materials would,
summed to give the wet concentration. in the long run, in the normal and correct operation of the test
The result may be converted from µg/mL to µg/g by: method exceed the following values only one case in twenty:
1.1
Repeatability 5 0.16 ~ X
!. (13)
total Aroclor ~ µg/mL!
Aroclor ~ µg/g ! 5 (10)
specific gravity of sample where X is the average PCB concentration in mg/kg.
14.1.2 Reproducibility—The difference between two single
Specific gravity may be the measured value or calculated by
and independent results obtained by different operators work-
(sample weight/3 mL).
ing in different laboratories on identical materials would in the
Care shall be taken in handling viscous samples as the
long run, exceed the following values only in one case in
volumes may not be correct. In those cases the measured
twenty.
sample weight shall be used.
A simplified formula using sample weight is: Reproducibility 5 0.73 ~ X 1.1! . (14)

Aroclor ~ µg/g, mg/Kg! 5 (11) where X is the average PCB concentration in mg/kg.
14.1.3 Precision estimates for selected values of X are set
total Aroclor ~ µg/mL! 3 out in the following Table 1:
dilution volume ~ mL! 3 additional dilution factor ~ mL/mL! 14.2 Bias—A reliable quantitation of bias was not possible
sample weight ~ g ! due to the manner in which the samples were prepared and
The concentration of Aroclor in a sample is corrected for dry aliquoted. However, the method tends to produce a result that
weight of the sample by the following: is low. This tendency is mitigated to some extent through the
use of a surrogate as described in Section 11.
Aroclor ~ mg/Kg! ~ wet!
Aroclor ~ mg/Kg! ~ dry! 5 (12)
~ 100 2 % water! /100 15. Keywords
13.4 Mixed Aroclors—For routine Tier II samples showing 15.1 gas chromatography; GC/ECD; PCBs; polychlorinated
evidence of mixed Aroclors, select a minimum of three peaks biphenyls
lacking significant interference for each identified Aroclor and 9
Supporting data have been filed at ASTM International Headquarters and may
quantitate. Report the amount for each Aroclor separately. be obtained by requesting Research Report RR:D02-1413.
NOTE 6—This approach will normally overstate the PCB concentration
and, thus, is considered to be a conservative approach. TABLE 1 Repeatability and Reproducibility
13.4.1 Since mixed Aroclors present special problems in X, mg/kg Repeatability Reproducibility
quantitation, it is permissible to prepare individualized mixed 5 0.9 4.3
standards in an attempt to match the suspected sample concen- 10 2.0 9.4
20 4.3 20.2
trations and obtain greatest possible accuracy. This will involve 50 11.8 55.5
a judgment about what proportion of the different suspected

8
 D6160 − 98 (2017)
ANNEXES

(Mandatory Information)

A1. POOR RECOVERY TROUBLESHOOTING

A1.1 If the necessary recovery is outside of limits, the A1.1.7 Re-evaluate surrogate standard.
following may be useful in identifying the source of the
problem: A1.2 If none of the above results in acceptable surrogate
recoveries:
A1.1.1 Check for proper dilution factor,
A1.1.2 Check for dirty insert and drifting baseline, A1.2.1 Break composites into individual samples, prepare
A1.1.3 Recheck the recovery calculation, samples, and reanalyze.
A1.1.4 Look for major interfering peak, A1.2.2 For individual samples, if the recovery is still
A1.1.5 Look for sample preparation problems, outside of the limits after a second preparation and analysis,
this demonstrates confirmation of a matrix effect and is
A1.1.6 Reanalyze sample, on different channel, if possible,
reported as such.
and

A2. SILYNIZATION

A2.1 There are many possible pathways to deactivate glass A2.3 Vapor Silynization
surfaces. These are basically divided into vapor and liquid
A2.3.1 Place the clean glass parts in a wide-mouth glass jar.
methods. Two examples follow:
A2.3.2 Add 1 mL of concentrated dimethyldichlorosilane to
A2.2 Liquid Silynization the jar.
A2.2.1 Prepare 5 % (volume) solution of dimethyldichlo- A2.3.3 Screw a lid on the jar and place it in an oven
rosilane in toluene. preheated to 50 °C for at least 2 h.
A2.2.2 Place the clean glass parts to be treated in a A2.3.4 Remove jar and open lid.
wide-mouth jar or beaker large enough to allow the solution to
cover the parts. A2.3.5 Rinse glass parts with methanol.
A2.2.3 Heat the solution with the glass part submerged to A2.3.6 Oven dry the glass parts at 100 °C for at least
the boiling point and continue gentle boiling for 30 min. 20 min.
A2.2.4 Allow the parts to drain and rinse with methanol. A2.4 Silanized glass parts shall be stored in the oven or in
A2.2.5 Oven dry the glass parts at 100 °C for at least a desiccator with activated desiccant in the bottom until
20 min. needed.

A3. COMPOSITING

A3.1 It is common to analyze mixtures of multiple samples, matrix to obtain a representative sample. Mix them well to get
called composites, if a large number of samples are analyzed. a composite of up to ten samples. If using the surrogate, be sure
Positive identification of PCBs within a composite usually then to consider the dilution factor.
requires that the individual samples making up the composite
A3.1.2 Compositing of Samples Representing Varying Vol-
be reanalyzed individually to identify the source of the PCBs. umes
A3.1.1 If samples are to be run as a composite, rather than A3.1.2.1 If receipt samples representing varying volumes
individually, transfer 1 mL of a representative portion of each (for example, multiple partially-filled drums) are to be
sample (1 g, if a solid) into a vial by means of disposable pipet. composited, it is important to ensure that each unit volume (for
Larger volumes than 1 mL may be used, if required by sample example, each litre) is equally represented. If preliminary

9
 D6160 − 98 (2017)
composites have been generated outside of the laboratory, the Assuming the 20 drum maximum is reached, place 20 mL of
analyst making the composite will need to understand the material in the vial. Vortex well.
volume of material represented by each sample.
A3.1.2.2 The composite is generated by using a pipette to A3.2 When Aroclor is detected in a composite at a level
transfer proportional amounts (for example, 1 mL ⁄drum) into a equal to or above the IPS, all samples included in the
vial. For example, if a sample entering the laboratory repre- composite shall be analyzed individually.
sents eight drums, place 8 mL of that sample in the vial.

A4. SAMPLE CLEAN-UP

A4.1 Clean-up is not required for all samples; however, the A4.4 Magnesium Silicate Column Clean-up:
following clean-up procedures will solve most interference A4.4.1 Plug a 10 mL disposable pipet with glass wool. Add
problems to obtain analyzable chromatograms. Use the par- the equivalent depth of 1 mL anhydrous sodium sulfate. Add
ticular clean-up method demonstrated to yield acceptable the equivalent depth of about 2 mL magnesium silicate. Top off
results, if a lab is familiar with the type of matrix in their the column with the equivalent depth of 1 mL anhydrous
samples. sodium sulfate. Tap the column gently. Optionally, one may use
A4.2 Magnesium Silicate Slurry and Acid Clean-Up (Indi- a commercial clean-up cartridge (1000 mg packing).
vidual Samples)—Pipet 1.0 mL of the 1:10 diluted A4.4.2 Put a container beneath the column to catch the
extract to a 20 mL vial containing 9.0 hexane. Further infor- eluate. Wet with 2 mL to 3 mL hexane. Transfer 1 mL to 2 mL
mation is provided in EPA Method 3620. of the acid cleaned sample to the column.
NOTE A4.1—For Composited Sample (see Annex A3)—No further
NOTE A4.2—Do not allow any acid to go into the column.
dilution required beyond the initial 1:10, unless sample matrix requires it.
Further dilutions may cause detection limits to rise above the level of A4.4.3 Discard the eluate. When the extract level reaches
interest. the top of the upper sodium sulfate, add 5 mL more of the
A4.2.1 Add 3 mL concentrated sulfuric acid to the solution. extract into the column. Collect the eluate in a GC autosampler
Cap it with a TFE-fluorocarbon-lined cap and vortex well. Let vial.
it settle to allow phase separation. More than one acid clean-up
A4.5 Combined Magnesium Silicate and Silica Gel Column
may be used if the acid layer is discolored after phase
Clean-up—Prepare a silica gel column using a 10 mL
separation. Record the number of washings performed.
disposable pipet plugged with glass wool. On top of the glass
A4.2.2 Transfer about 8 mL of this solution (free from acid) wool place 1 mL silica gel. Add to the column about 1 mL
into another 20 mL vial, containing about 0.25 g magnesium magnesium silicate and then 1 mL anhydrous sodium sulfate.
silicate and 0.5 g of anhydrous sodium sulfate. For used oil Tap the column gently. Transfer 5 mL of already acid cleaned
samples it may be preferable to use 0.25 g anhydrous sodium sample to wet column (see EPA Method 3620)
sulfate and 0.5 g silica gel. Vortex well and allow the magne-
A4.5.1 Discard the eluate. When the extract level reaches
sium silicate to settle by gently tapping the vial or by
the top of the upper sodium sulfate, add about 3 mL more of
centrifuging for about 2 min.
the extract. Collect about 2 mL in a GC vial.
A4.2.3 The final solution after clean-up is transferred into a
GC vial. A4.6 Copper Clean-Up —Elemental sulfur in samples will
cause interferences in the GC/ECD analysis. Presence of sulfur
A4.3 Silica Gel Slurry Clean-Up—Follow the procedure for will be indicated by a yellow extract color and big interfering
magnesium silicate clean-up, substituting silica gel for magne- peaks. Check sample history for the presence of sulfur. To
sium silicate. Samples that have undergone acid clean-up and remove the sulfur, transfer as much as possible of the extract
magnesium silicate slurry and that still display interferences (usually 7 mL to 8 mL) into a vial, add 0.5 g powdered copper;
shall undergo an additional silica gel slurry cleanup. The seal, and vortex vigorously. Allow the copper sulfide to settle.
extract, after acid and magnesium silicate slurry clean-up, is Remove about 4 mL of the hexane solution and perform an
pipetted to a 20 mL vial containing 0.5 g silica gel and acid wash, if needed, to clear the hexane phase. Further
vortexed. Further information can be found in EPA Method information can be found in EPA Method 3660. (Warning—
3630. Handle mercury with care. Keep a minimum amount on site.)

10
 D6160 − 98 (2017)
APPENDIXES

(Nonmandatory Information)

X1. EXAMPLE CALIBRATION TABLE AND CHROMATOGRAM

X1.1 See Table X1.1 for an example calibration table and X1.2.2 The decachlorobiphenyl surrogate internal standard
chromatogram. is also shown and designated as 15.220–DCB.
X1.2 Chromatogram X1.2.3 This chromatogram was generated using the longer
X1.2.1 The chromatogram in Fig. X1.1 includes the reten- run time described in 10.1.2.
tion time in minutes for each major peak in a mixture of
Aroclors 1016 and 1260. The five peaks for each Aroclor used
for quantitation are clearly marked (for example, 7.295–1016).

TABLE X1.1 Calibration Table

Retention Peak Average Standard Peak
Time Name Response Deviation % RSD
7.520 1016 4543228 528055 11.62
7.870 1016 2743429 214966 7.84
8.390 1016 6378927 360623 5.65
10.150 1016 1851507 129351 6.99
10.540 1016 1919245 150403 7.84
11.540 1260 4325072 493032 11.40
11.930 1260 6012570 639705 10.64
12.370 1260 5503749 470809 8.57
13.430 1260 5830717 428980 7.36
13.880 1260 3118738 164338 5.27

11
12
D6160 − 98 (2017)

FIG. X1.1 Sample Chromatogram

 D6160 − 98 (2017)

X2. WORKSHEETS

X2.1 See Fig. X2.1 and Fig. X2.2 for calculation work-
sheets.

FIG. X2.1 PCB Calculation Work Sheet for Spikes

13
 D6160 − 98 (2017)

FIG. X2.2 AROCLOR Calculation Work Sheet

14
 D6160 − 98 (2017)
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15