ASTM D5384-11
(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
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.
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 Bromide and iodide are also titrated and reported on a molar basis as chlorine.
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 to 1180 mg/kg5.
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.6This 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.
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Designation: D5384 − 11
StandardTest 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* responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 These test methods cover the determination of chlorine
bility of regulatory limitations prior to use. Specific safety
in used oils, fuels, and related materials, including: crankcase,
statements are given in Sections 3, 6, and 7.
hydraulic, diesel, lubricating and fuel oils, and kerosene, all
containing <25 % (mass/mass) water.
2. Referenced Documents
1.1.1 Bromide and iodide are also titrated and reported on a
2
2.1 ASTM Standards:
molar basis as chlorine.
D4057 Practice for Manual Sampling of Petroleum and
1.2 The entire analytical sequence, including sampling,
Petroleum Products
sample pretreatment, chemical reactions, extraction, and
quantification, is available in kit form using predispensed and
3. Summary of Test Methods
encapsulated reagents. The overall objective is to provide a
3.1 The oil sample (approximately 0.3 g) is dispersed in a
simple, easy to use procedure, permitting nontechnical person-
hydrocarbon solvent and reacted with a mixture of metallic
neltoperformatestinoroutsideofthelaboratoryenvironment
sodium catalyzed with naphthalene and diglyme at ambient
in under 10 min. The test method also gives information to run
temperature. This process converts organic halogens to their
the test without a kit.
respective sodium halides. Halides in the treated mixture,
1.2.1 Test Method A is preset to provide a greater than or
including those present prior to the reaction, are then extracted
less than result at 1000 mg/kg (ppm) total chlorine to meet
into an aqueous buffer, which is then titrated with mercuric
regulatory requirements for used oils.
nitrateusingdiphenylcarbazoneastheindicator.Theendpoint
1.2.2 Test Method B provides results over a range from 200
of the titration is the formation of the blue-violet mercury
to 4000 mg/kg total chlorine.
diphenylcarbazone complex.
1.3 For both test methods, positive bias will result from
3.1.1 PresetreagentquantitiesareusedforTestMethodAso
samples that contain greater than 3 % (mass/mass) total sulfur.
that the final result is clearly determined to be either above or
While a false negative result will not occur, other analytical
below 1000 mg/kg total chlorine.
methods should be used on high sulfur oils.
3.1.2 A fixed concentration titrant of mercuric nitrate in
waterisusedforTestMethodB.Atitrationisperformedonthe
1.4 Test Method B, Lower Limit of Quantitation—In the
extracted aqueous sample until the color changes from yellow
round-robin study to develop statistics for this test method,
to blue. At this point, the titration is stopped and the chlorine
participants were asked to report results to the nearest 100
concentration is determined based on the volume of titrant
mg/kg. The lower limit of quantification could therefore only
5
added. (Warning—In case of accidental breakage onto skin or
be determined to be in the range from 870 to 1180 mg/kg .
clothing,washwithlargeamountsofwater.Allthereagentsare
1.5 The values stated in SI units are to be regarded as
poisonousandshouldnotbetakeninternally.)(Warning—The
standard. No other units of measurement are included in this
gray ampules contain metallic sodium which is a flammable,
standard.
water-reactive solid. Reaction with water will generate flam-
1.6 This standard does not purport to address all of the
mable hydrogen gas.) (Warning—In addition to other
safety concerns, if any, associated with its use. It is the
precautions, do not ship kits on passenger aircraft. Kits contain
metallic sodium and mercury salts. Used kits will pass the
USEPAToxic Characteristic Leaching Procedure (TCLP) test.
1
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
2
tee D02.03 on Elemental Analysis. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
CurrenteditionapprovedJune1,2011.PublishedJuly2011.Originallyapproved contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
in 1995. Last previous edition approved in 2005 as D5384–95(2005). DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5384–11. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D5384–95 (Reapproved 2005) Designation:D5384–11
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 Bromide and iodide are also titrated and reported on a molar basis as chlorine.
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 MethodAis 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
5
in the range from 870 to 1180 mg/kg .
1.5The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
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
3. Summary of Test Methods
3.1 The oil sample (approximately 0.3 g) is dispersed in a hydrocarbon solvent and reacted with a mixture of metallic sodium
catalyzedwithnaphthaleneanddiglymeatambienttemperature.Thisprocessconvertsorganichalogenstotheirrespectivesodium
halides. Halides in the treated mixture, including those present prior to the reaction, are then extracted into an aqueous buffer,
whichisthentitratedwithmercuricnitrateusingdiphenylcarbazoneastheindicator.Theendpointofthetitrationistheformation
of the blue-violet mercury diphenylcarbazone complex.
3.1.1 Preset reagent quantities are used for Test Method A so that the final result is clearly determined to be either above or
below 1000 mg/kg total chlorine.
3.1.2 A fixed concentration titrant of mercuric nitrate in water is used for Test Method B. A titration is performed on the
extracted aqueous sample until the color changes from yellow to blue. At this point, the titration is stopped and the chlorine
concentrationisdeterminedbasedonthevolumeoftitrantadded.(Warning—Incaseofaccidentalbreakageontoskinorclothing,
1
These test methods are under the jurisdiction ofASTM Committee D02 on Petroleum Products and Lubricants and are the direct responsibility of Subcommittee D02.03
on Elemental Analysis.
´1
Current edition approved May 1, 2005. Published May 2005. Originally approved in 1995. Last previous edition approved in 2000 as D5384–95(2000) . DOI:
10.1520/D5384-95R05.
Current edition approved June 1, 2011. Published July 2011. Originally approved in 1995. Last previous edition approved in 2005 as D5384–95(2005). DOI:
10.1520/D5384–11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book ofASTM Standards
volume information, r
...
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