ASTM D5384-95(2000)e1
(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)
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 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 Method B provides results over a range from 200 to 4000 mg/kg total chlorine.
1.3 For both 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 Method B Lower Limit of Quantitation -In the round- robin study to develop statistics for this 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/kg .
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.6 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 Section 3.
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An American National Standard
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Designation:D5384–95 (Reapproved 2000)
Standard Test Methods for
Chlorine in Used Petroleum Products (Field Test Kit
Method)
This standard is issued under the fixed designation D 5384; 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.
e NOTE—Warning notes were made part of the text in April 2000.
1. Scope bility of regulatory limitations prior to use. Specific safety
statements are given in Sections 3 and 6.
1.1 These test methods cover the determination of chlorine
in used oils, fuels, and related materials, including: crankcase,
2. Referenced Documents
hydraulic, diesel, lubricating and fuel oils, and kerosene, all
2.1 ASTM Standards:
containing <25 % (mass/mass) water.
D 4057 Practice for Manual Sampling of Petroleum and
1.1.1 Bromide and iodide are also titrated and reported on a
Petroleum Products
molar basis as chlorine.
1.2 The entire analytical sequence, including sampling,
3. Summary of Test Methods
sample pretreatment, chefru
3.1 The oil sample (approximately 0.3 g) is dispersed in a
mical reactions, extraction, and quantification, is available in
hydrocarbon solvent and reacted with a mixture of metallic
kit form using predispensed and encapsulated reagents. The
sodium catalyzed with naphthalene and diglyme at ambient
overall objective is to provide a simple, easy to use procedure,
temperature. This process converts organic halogens to their
permitting non-technical personnel to perform a test in or
respective sodium halides. Halides in the treated mixture,
outsideofthelaboratoryenvironmentinunder10min.Thetest
including those present prior to the reaction, are then extracted
method also gives information to run the test without a kit.
into an aqueous buffer, which is then titrated with mercuric
1.2.1 Method A is preset to provide a greater than or less
nitrateusingdiphenylcarbazoneastheindicator.Theendpoint
than result at 1000 mg/kg (ppm) total chlorine to meet
of the titration is the formation of the blue-violet mercury
regulatory requirements for used oils.
diphenylcarbazone complex.
1.2.2 Method B provides results over a range from 200 to
3.1.1 Preset reagent quantities are used for MethodAso that
4000 mg/kg total chlorine.
thefinalresultisclearlydeterminedtobeeitheraboveorbelow
1.3 For both methods, positive bias will result from samples
1000 mg/kg total chlorine.
that contain greater than 3 % (mass/mass) total sulfur. While a
3.1.2 A fixed concentration titrant of mercuric nitrate in
false negative result will not occur, other analytical methods
water is used for Method B. A titration is performed on the
should be used on high sulfur oils.
extracted aqueous sample until the color changes from yellow
1.4 Method B Lower Limit of Quantitation—In the roun-
to blue. At this point, the titration is stopped and the chlorine
drobin study to develop statistics for this method, participants
concentration is determined based on the volume of titrant
were asked to report results to the nearest 100 mg/kg. The
added. (Warning—In case of accidental breakage onto skin or
lower limit of quantification could therefore only be deter-
5 clothing,washwithlargeamountsofwater.Allthereagentsare
mined to be in the range from 870 to 1180 mg/kg .
poisonousandshouldnotbetakeninternally.)(Warning—The
1.5 The values stated in SI units are to be regarded as the
gray ampules contain metallic sodium which is a flammable,
standard. The values given in parentheses are for information
water-reactive solid. Reaction with water will generate flam-
only.
mable hydrogen gas.) (Warning—In addition to other precau-
1.6 This standard does not purport to address all of the
tions, do not ship kits on passenger aircraft. Kits contain
safety concerns, if any, associated with its use. It is the
metallic sodium and mercury salts. Used kits will pass the
responsibility of the user of this standard to establish appro-
USEPAToxic Characteristic Leaching Procedure (TCLP) test.
priate safety and health practices and determine the applica-
Check with your state environmental enforcement office to see
if additional disposal regulations may apply.) (Warning—
When the sodium ampule in either kit is crushed, oils that
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
tee D02.03 on Elemental Analysis.
Current edition approved Aug. 15, 1995. Published October 1995. Annual Book of ASTM Standards, Vol 05.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5384–95 (2000)
contain more than 25 % (m/m) water will cause the sample to 6.2 If not using prepackaged kits, the following must be
turn clear to light gray and will build noticeable pressure. prepared.
Under these circumstances, the results can be biased exces- 6.2.1 A solution of 10 % (m/m) naphthalene in bis-2-
sively low and should be disregarded. (Warning—In addition methoxy-ethyl ether (diglyme). Dissolve 10 g of naphthalene
to other precautions, take care to ensure that fingers are not cut into 90 g of bis-2-methoxy-ethyl ether.
by glass in the kits. All reagents in pre-packaged kits are 6.2.2 Adispersion of 40 % (m/m) ground sodium in mineral
contained in crushable glass ampules inside plastic test tubes. oil.
Each ampule should be crushed only once to reduce the risk of 6.2.3 A0.15 % (mass/volume) solution of s-diphenyl carba-
glass pieces piercing the sides of the tube. Wear safety glasses zone in ethyl alcohol. Dissolve 0.15 g s-diphenyl carbazone
and gloves throughout the testing procedure.) powder into 100 mL of ethyl alcohol.
6.2.4 For Method A, a 4.75-mmol/L solution of mercuric
4. Significance and Use
nitrate. Prepare a mercuric nitrate stock solution by first
dissolving 5.14 g Hg(NO ) ·HO(WARNING-
4.1 Chlorinated compounds can lead to corrosion of equip- 3 2 2
EXTREMELYTOXIC) in 5 mLof 50 % (vol/vol) nitric acid.
ment and poisoning of the catalyst. Chlorinated compounds
Aftersolutehascompletelydissolved,makeupto150mLwith
also present a health hazard when incompletely combusted.
Type II water. Stock solution = 0.100 mol/L. Prepare 4.75
Chlorine content of petroleum products is determined prior to
mmol/L solution by putting 47.5 mL of stock solution into a
their being recycled.
1-L volumetric flask and make up to 1 L with Type II water.
NOTE 1—Federal Regulations mandate that often the chlorine content
6.2.5 For Method B, a 13.7-mmol/L solution of mercuric
of used oil must be determined before recycling.
nitrate. Place 137 mL of stock solution (see 6.2.4) into a 1-L
4.2 These test methods can be used to determine when a
volumetric flask and make up to 1 L with Type II water.
usedpetroleumproductmeetsorexceedsrequirementsfortotal
6.2.6 An aqueous buffer solution containing 6 % (mass/
halogens measured as chloride. It is specifically designed for
mass) sodium sulfate, 2.6 % (mass/mass) sodium phosphate
used oils, permitting on-site testing at remote locations by
and 3.175 % (mass/mass) sulfuric acid (pH 1.5).
nontechnical personnel to avoid the delays of laboratory
7. Sampling
testing.
7.1 Take samples in accordance with the instructions in
5. Apparatus
Practice D 4057.
5.1 Both the fixed end point test (Method A) and the 7.2 Free water, as a second phase, is to be removed.
quantitative test (Method B) are available as completely However, this second phase can be analyzed separately for
self-contained test kits containing all the reagents necessary to chloride content by using a method suitable for materials with
high water content (Warning—The gray ampules contain
complete the test. Each kit includes a sampling syringe to
withdraw a fixed volume of sample for analysis; a first metallic sodium which is a flammable, water-reactive solid.
Reaction with water will generate flammable hydrogen gas.)
polyethylene test tube into which the sample is introduced for
dilution and reaction with metallic sodium; a second polyeth- (Warning—When the sodium ampule in either kit is crushed,
oils that contain more than 25 % (m/m) water will cause the
ylene tube containing a buffered aqueous extractant, the
mercuric nitrate titrant (Method A only), and diphenyl carba- sample to turn clear to light gray and will build noticea
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