Standard Test Method for Analysis of Polychlorinated Biphenyls in Insulating Liquids by Gas Chromatography

SIGNIFICANCE AND USE
5.1 United States governmental regulations mandate that electrical apparatus and electrical insulating fluids containing PCB be handled and disposed of through specific procedures. The procedure to be used for a particular apparatus or quantity of insulating fluid is determined by the PCB content of the fluid. The results of this analytical technique can be useful in selecting the appropriate handling and disposal procedure.  
5.2 Quantification in this technique requires a peak-by-peak comparison of the chromatogram of an unknown specimen with that of standard Aroclor test specimens obtained under identical conditions. The amount of PCB producing each peak in the standard chromatogram shall be known independently.  
5.3 The technique described is based on data for standard chromatograms of Aroclors 1242, 1254, and 1260 obtained using specific chromatographic column packing materials and operating conditions.4 Relevant chromatograms are reproduced in Fig. 1, Fig. 2, and Fig. 35, for isothermal packed columns and in Figs. X4.1 through X4.3) for temperature programmed mega-bore capillary columns. Each peak is identified by its retention time relative to that of a standard. The types and amounts of PCB associated with each peak have been determined by mass spectroscopy and are given in Table 1, Table 2, and Table 3.4 Other chromatographic operating conditions, and in particular, other column packing materials, may give different separations. The data given in the tables should not be used if chromatograms of the standards differ significantly from those shown in the figures. The peaks in such standard chromatograms shall be independently identified and quantified.  
5.4 Different isomers of PCB with the same number of chlorine substituents can cause substantially different responses from EC detectors. Mixtures of PCB containing the same amount of PCB, but with a different ratio of isomers, can give quite different chromatograms. This technique is effective only when...
SCOPE
1.1 This test method describes a quantitative determination of the concentration of polychlorinated biphenyls (PCBs) in electrical insulating liquids by gas chromatography. It also applies to the determination of PCB present in mixtures known as askarels, used as electrical insulating liquids.  
1.2 The PCB mixtures known as Aroclors2 were used in the formulation of the PCB-containing askarels manufactured in the United States. This test method may be applied to the determination of PCBs in insulating liquids contaminated by either individual Aroclors or mixtures of Aroclors. This technique may not be applicable to the determination of PCBs from other sources of contamination.  
1.3 The precision and bias of this test method have been established only for PCB concentrations in electrical insulating mineral oils and silicones. The use of this test method has not been demonstrated for all insulating fluids. Some insulating liquids, such as halogenated hydrocarbons, interfere with the detection of PCBs and cannot be tested without pretreatment.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

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30-Nov-2018
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ASTM D4059-00(2018) - Standard Test Method for Analysis of Polychlorinated Biphenyls in Insulating Liquids by Gas Chromatography
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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: D4059 − 00 (Reapproved 2018)
Standard Test Method for
Analysis of Polychlorinated Biphenyls in Insulating Liquids
1
by Gas Chromatography
This standard is issued under the fixed designation D4059; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
3
2.1 ASTM Standards:
1.1 This test method describes a quantitative determination
of the concentration of polychlorinated biphenyls (PCBs) in D923Practices for Sampling Electrical Insulating Liquids
electrical insulating liquids by gas chromatography. It also
3. Symbols
appliestothedeterminationofPCBpresentinmixturesknown
as askarels, used as electrical insulating liquids.
3.1 The following symbols are used in this test method:
2
C —concentration of PCB (ppm by weight) in the insulating test specimen.
1.2 The PCB mixtures known asAroclors were used in the
C —concentration of PCB (ppm by weight) found for the peak, i,inthe
i
formulation of the PCB-containing askarels manufactured in
chromatogram of the insulating liquid test specimen.
the United States. This test method may be applied to the
d —density of the test specimen at 25°C, g/mL.
f —relative content of the PCB species associated with each individual
determination of PCBs in insulating liquids contaminated by
i
peak, i, in the chromatogram of the standard Aroclor solution, %.
either individual Aroclors or mixtures of Aroclors. This tech-
M —total amount of PCB in the standard test specimen injected into the
niquemaynotbeapplicabletothedeterminationofPCBsfrom
chromatograph, g.
M —amount of PCB represented by peak, i, in the chromatogram of the
other sources of contamination.
i
standard Aroclor test specimen, g.
s
1.3 The precision and bias of this test method have been R —response of the detector to PCB components with relative retention
i
time, i, in the chromatograms of the standard, s, solutions, response
establishedonlyforPCBconcentrationsinelectricalinsulating
may be expressed as peak height, peak area, or integrator counts.
mineral oils and silicones. The use of this test method has not x
R —response of the detector to PCB components with relative retention
i
time, i, in the chromatogram of an unknown test specimen, may be
been demonstrated for all insulating fluids. Some insulating
expressed as peak height, peak area, or integrator counts.
liquids, such as halogenated hydrocarbons, interfere with the
s
R —response of the detector to PCB components in the largest or most
p
detection of PCBs and cannot be tested without pretreatment.
cleanly separated peaks, p, in chromatograms of standard solutions;
may be expressed as peak height, peak area, or integrator counts.
1.4 The values stated in SI units are to be regarded as
x
R —response of the detector to PCB components in the largest or most
p
standard. No other units of measurement are included in this cleanly separated peaks, p, in the chromatogram of an unknown test
specimen contaminated by a single Aroclor; may be expressed in
standard.
peak height, peak area, or integrator counts.
s
1.5 This standard does not purport to address all of the ν —volume of the standard test specimen injected into the
chromatograph, µL.
safety concerns, if any, associated with its use. It is the
x
ν —volume of the unknown test specimen injected into the
responsibility of the user of this standard to establish appro-
chromatograph, µL.
V —original volume of the test specimen to be analyzed, µL.
priate safety, health, and environmental practices and deter-
s
V —total volume of the diluted standard, mL.
mine the applicability of regulatory limitations prior to use.
x
V —total volume of the test specimen to be analyzed, µL.
x
1.6 This international standard was developed in accor-
W —weight of the test specimen to be analyzed, g.
s
W —weight of the initial standard Aroclor test specimen, g.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4. Summary of Test Method
Development of International Standards, Guides and Recom-
4.1 Thetestspecimenisdilutedwithasuitablesolvent.The
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. resulting solution is treated by a procedure to remove interfer-
ing substances after which a small portion of the resulting
solution is injected into a gas chromatographic column. The
componentsareseparatedastheypassthroughthecolumnwith
1
This
...

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