ASTM D5384-14
(Test Method)Standard Test Methods for Chlorine in Used Petroleum Products (Field Test Kit Method)
Standard Test Methods for Chlorine in Used Petroleum Products (Field Test Kit Method)
SIGNIFICANCE AND USE
4.1 Chlorinated compounds can lead to corrosion of equipment and poisoning of the catalyst. Chlorinated compounds also present a health hazard when incompletely combusted. Chlorine content of petroleum products is determined prior to their being recycled.
Note 1: Federal Regulations mandate that often the chlorine content of used oil must be determined before recycling. EPA regulation 40 CFR 261 bars the sale of used oil for fuel if it is contaminated with halogens measured as chlorine at levels exceeding 1000 mg/kg. Such oil is considered to be a hazardous waste unless it can be proven that the chlorine content is inorganic or that the halogenated organics are not hazardous constituents. The cost of disposing of a hazardous waste is many times higher than the cost of used oil disposal. Therefore it is critical for users, generators, haulers, reprocessors, and collectors to test the material they handle in order to comply with regulations, maintain safe operations, and avoid high disposal costs.
4.2 These test methods can be used to determine when a used petroleum product meets or exceeds requirements for total halogens measured as chloride. It is specifically designed for used oils, permitting on-site testing at remote locations by nontechnical personnel to avoid the delays of laboratory testing.
SCOPE
1.1 These test methods cover the determination of chlorine in used oils, fuels, and related materials, including: crankcase, hydraulic, diesel, lubricating and fuel oils, and kerosene, all containing
1.1.1 If the sample contains greater than 25 % water, the sodium metal reacts preferentially with the water rather than with the halogenated organics in the oil.
1.1.2 Bromide and iodide are also titrated and reported on a molar basis as chlorine. The method does not detect fluorine because AgF remains in the solution during the titration, while AgI, AgBr, and AgCl precipitate out and can therefore be detected.
1.1.3 Some of the chlorinated organic compounds that have been shown to be detectable by this method include trichloroethane, dichloroethane, trichlorobenzene, monochlorobenzene, chlorooctadecane, methylene chloride, perchloroethylene, Freon, and polychlorinated biphenyls. These nine compounds represent the major classes of chlorinated compounds that are found in used oils.
1.2 The entire analytical sequence, including sampling, sample pretreatment, chemical reactions, extraction, and quantification, is available in kit form using predispensed and encapsulated reagents. The overall objective is to provide a simple, easy to use procedure, permitting nontechnical personnel to perform a test in or outside of the laboratory environment in under 10 min. The test method also gives information to run the test without a kit.
1.2.1 Test Method A is preset to provide a greater than or less than result at 1000 mg/kg (ppm) total chlorine to meet regulatory requirements for used oils.
1.2.2 Test Method B provides results over a range from 200 to 4000 mg/kg total chlorine.
1.3 For both test methods, positive bias will result from samples that contain greater than 3 % (mass/mass) total sulfur. While a false negative result will not occur, other analytical methods should be used on high sulfur oils.
1.4 Test Method B, Lower Limit of Quantitation—In the round-robin study to develop statistics for this test method, participants were asked to report results to the nearest 100 mg/kg. The lower limit of quantification could therefore only be determined to be in the range from 870 mg/kg5 to 1180 mg/kg5.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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 and health practices and determine the applicability of re...
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Designation: D5384 − 14
Standard Test Methods for
Chlorine in Used Petroleum Products (Field Test Kit
1
Method)
This standard is issued under the fixed designation D5384; 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* While a false negative result will not occur, other analytical
methods should be used on high sulfur oils.
1.1 These test methods cover the determination of chlorine
in used oils, fuels, and related materials, including: crankcase, 1.4 Test Method B, Lower Limit of Quantitation—In the
hydraulic, diesel, lubricating and fuel oils, and kerosene, all round-robin study to develop statistics for this test method,
containing <25 % (mass/mass) water. participants were asked to report results to the nearest
1.1.1 If the sample contains greater than 25 % water, the 100 mg⁄kg. The lower limit of quantification could therefore
5
sodium metal reacts preferentially with the water rather than only be determined to be in the range from 870 mg⁄kg to
5
with the halogenated organics in the oil. 1180 mg⁄kg .
1.1.2 Bromide and iodide are also titrated and reported on a
1.5 The values stated in SI units are to be regarded as
molar basis as chlorine. The method does not detect fluorine
standard. No other units of measurement are included in this
becauseAgF remains in the solution during the titration, while
standard.
AgI, AgBr, and AgCl precipitate out and can therefore be
1.6 This standard does not purport to address all of the
detected.
safety concerns, if any, associated with its use. It is the
1.1.3 Some of the chlorinated organic compounds that have
responsibility of the user of this standard to establish appro-
been shown to be detectable by this method include
priate safety and health practices and determine the applica-
trichloroethane, dichloroethane, trichlorobenzene,
bility of regulatory limitations prior to use. Specific safety
monochlorobenzene, chlorooctadecane, methylene chloride,
statements are given in Sections 3, 6, and 7.
perchloroethylene, Freon, and polychlorinated biphenyls.
These nine compounds represent the major classes of chlori-
2. Referenced Documents
nated compounds that are found in used oils.
2
2.1 ASTM Standards:
1.2 The entire analytical sequence, including sampling,
D4057 Practice for Manual Sampling of Petroleum and
sample pretreatment, chemical reactions, extraction, and
Petroleum Products
quantification, is available in kit form using predispensed and
2.2 Federal Regulation:
encapsulated reagents. The overall objective is to provide a
3
40 CFR 261 Identification and Listing of Hazardous Waste
simple, easy to use procedure, permitting nontechnical person-
neltoperformatestinoroutsideofthelaboratoryenvironment
3. Summary of Test Methods
in under 10 min. The test method also gives information to run
3.1 The oil sample (approximately 0.3 g) is dispersed in a
the test without a kit.
hydrocarbon solvent and reacted with a mixture of metallic
1.2.1 Test Method A is preset to provide a greater than or
sodium catalyzed with naphthalene and diglyme at ambient
less than result at 1000 mg/kg (ppm) total chlorine to meet
temperature. This process converts organic halogens to their
regulatory requirements for used oils.
respective sodium halides. Halides in the treated mixture,
1.2.2 Test Method B provides results over a range from 200
including those present prior to the reaction, are then extracted
to 4000 mg/kg total chlorine.
into an aqueous buffer, which is then titrated with mercuric
1.3 For both test methods, positive bias will result from
nitrateusingdiphenylcarbazoneastheindicator.Theendpoint
samples that contain greater than 3 % (mass/mass) total sulfur.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
These test methods are under the jurisdiction of ASTM Committee D02 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Petroleum Products, Liquid Fuels, and Lubricants and are the direct responsibility Standards volume information, refer to the standard’s Document Summary page on
of Subcommittee D02.03 on Elemental Analysis. the ASTM website.
3
CurrenteditionapprovedJune1,2014.PublishedJuly2014.Originallyapproved AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
in 1995. Last previous edition approved in 2011 as D5384 – 11. DOI: 10.1520/ 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
D5384–14. www.access.gpo.gov.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5384 − 11 D5384 − 14
Standard Test Methods for
Chlorine in Used Petroleum Products (Field Test Kit
1
Method)
This standard is issued under the fixed designation D5384; 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 These test methods cover the determination of chlorine in used oils, fuels, and related materials, including: crankcase,
hydraulic, diesel, lubricating and fuel oils, and kerosene, all containing <25 % (mass/mass) water.
1.1.1 If the sample contains greater than 25 % water, the sodium metal reacts preferentially with the water rather than with the
halogenated organics in the oil.
1.1.2 Bromide and iodide are also titrated and reported on a molar basis as chlorine. The method does not detect fluorine because
AgF remains in the solution during the titration, while AgI, AgBr, and AgCl precipitate out and can therefore be detected.
1.1.3 Some of the chlorinated organic compounds that have been shown to be detectable by this method include trichloroethane,
dichloroethane, trichlorobenzene, monochlorobenzene, chlorooctadecane, methylene chloride, perchloroethylene, Freon, and
polychlorinated biphenyls. These nine compounds represent the major classes of chlorinated compounds that are found in used oils.
1.2 The entire analytical sequence, including sampling, sample pretreatment, chemical reactions, extraction, and quantification,
is available in kit form using predispensed and encapsulated reagents. The overall objective is to provide a simple, easy to use
procedure, permitting nontechnical personnel to perform a test in or outside of the laboratory environment in under 10 min. The
test method also gives information to run the test without a kit.
1.2.1 Test Method A is preset to provide a greater than or less than result at 1000 mg/kg (ppm) total chlorine to meet regulatory
requirements for used oils.
1.2.2 Test Method B provides results over a range from 200 to 4000 mg/kg total chlorine.
1.3 For both test methods, positive bias will result from samples that contain greater than 3 % (mass/mass) total sulfur. While
a false negative result will not occur, other analytical methods should be used on high sulfur oils.
1.4 Test Method B, Lower Limit of Quantitation—In the round-robin study to develop statistics for this test method, participants
were asked to report results to the nearest 100100 mg mg/kg. ⁄kg. The lower limit of quantification could therefore only be
5 5
determined to be in the range from 870870 mg ⁄kg to 1180 1180 mg mg/kg⁄kg .
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific safety statements are given in Sections 3, 6, and 7.
2. Referenced Documents
2
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
2.2 Federal Regulation:
3
40 CFR 261 Identification and Listing of Hazardous Waste
1
These test methods are under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and are the direct responsibility
of Subcommittee D02.03 on Elemental Analysis.
Current edition approved June 1, 2011June 1, 2014. Published July 2011July 2014. Originally approved in 1995. Last previous edition approved in 20052011 as
D5384–95(2005).D5384 – 11. DOI: 10.1520/D5384–11.10.1520/D5384–14.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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D5384 − 14
3. Summary of T
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